MOXIFLOXACIN

MOXIFLOXACIN

syn.......http://newdrugapprovals.org/2014/02/19/moxifloxacin-bay-12-8039/
1H NMR AND 13C IN DMSO.D6

13C ASSIGN


 



 


1H NMR ASSIGN

 

syn.......http://newdrugapprovals.org/2014/02/19/moxifloxacin-bay-12-8039/

Vietnam Journal of Chemistry

DOI: 10.15625/0866-7144.2015-2e-012

A practical synthesis of fluoroquinolone antibiotic moxifloxacin

Le Nguyen Thanh, Tran Huu Giap, To Hai Tung, Nguyen Anh Dung, Van Thi My Hue, Cao Thi Hue, Nguyen Thi Minh Hang, Nguyen Van Hung, Chau Van Minh

http://vjs.ac.vn/index.php/vjchem/article/view/0866-7144.2015-2e-012

206-208 oC;

1H-NMR
(500 MHz, DMSO-d6) δ (ppm): 8.62 (s, 1H, H-2);
7.60 (d, J = 14.5 Hz, 1H, H-5); 4.12-4.10 (m, 1H, H-
13); 3.98-3.94 (m, 1H); 3.88-3.86 (m, 1H); 3.54 (s,
3H, H-12); 3.37-3.23 (m, 3H); 2.88-2.86 (m, 1H);
2.54-2.51(m, 1H); 2.24 (m, 1H); 1.73- 1.59 (m, 3H);
1.41 (m, 1H); 1.21-1.17 (m, 1H); 1.13-1.08 (m, 1H);
1.02-0.96 (m, 1H); 0.89-0.84 (m, 1H).

13C-NMR
(125MHz, DMSO-d6) δ (ppm): 175.8; 165.9; 153.7;
149.9; 140.2; 137.3; 134.5; 116.4; 106.3; 106.1;
61.1; 58.5; 56.0; 52.1; 44.4; 40.6; 36.3; 22.9; 21.5;
9.6; 8.1. ESI-MS m/z: [M-H]-: 400.


 


COSY

• Figure 13A: X-ray powder diffraction pattern of Moxifloxacin hydrochloride methylene dichloride solvate.
• Figure 13B: Infrared spectrum of Moxifloxacin hydrochloride methylene dichloride solvate.

 

• Figure 13C: ¹H-NMR spectrum (DMSO-d6, TMS) of Moxifloxacin hydrochloride methylene dichloride solvate.

 

• Figure 14A: X-ray powder diffraction pattern of anhydrous Moxifloxacin hydrochloride form IV.
• Figure 14B: Infrared spectrum of anhydrous Moxifloxacin hydrochloride form IV.

 

• Figure 15A: X-ray powder diffraction pattern of Moxifloxacin hydrochloride acetic acid solvate.
• Figure 15B: Infrared spectrum of Moxifloxacin hydrochloride acetic acid solvate.

 

• Figure 15C: 1H-NMR spectrum (DMSO-d6, TMS) of Moxifloxacin hydrochloride acetic acid solvate.

 

• Figure 16A: X-ray powder diffraction pattern of Moxifloxacin hydrochloride nitromethane solvate.
• Figure 16B: Infrared spectrum of Moxifloxacin hydrochloride nitromethane solvate.

 

syn.......http://newdrugapprovals.org/2014/02/19/moxifloxacin-bay-12-8039/

• Figure 16C: 1H-NMR spectrum (DMSO-d6, TMS) of Moxifloxacin hydrochloride nitromethane solvate.

.
 

Example 13

preparation of Moxifloxacine hydrochloride anhydrous form IVExample13.aMoxifloxacine hydrochloride methylene dichloride solvate
• [0100]
  5 g (12,5 mmol) Moxifloxacin were prepared according to EP 550903 and dissolved in 50 ml methylene dichloride at room temperature. To this solution 0,9 ml (1,2 equiv.) acetic acid and 2 ml (1,2 equiv.) trimethylchlorosilane were added under stirring. Immediately after addition of the chlorosilane the crystallization started. The suspension was stirred for about 30 min and the precipitate filtered off and dried under vacuum at room temperature to yield 6,3g (94,2%) of the 1:1 solvate of Moxifloxacine hydrochloride with methylene dichloride.
  ¹H-NMR (DMSO-d₆): 0.8 - 0.95 (m, 1H), 0.95 - 1.3 (m, 3H), 1.6 - 1.9 (m, 4 H), 2.55 - 2.75 (m, 1H), 2.8 - 3.0 (m, 1H), 3.5 - 3.7 (m with Singlet at 3.6 ppm, 4H), 3.7 - 3.8 (m, 1H), 3.8 - 4.0 (m, 2H), 4.0 - 4.2 (m, 2H), 5.77 (s, 2H), 7.65 (d, J = 14 Hz, 1H), 8.66 (s, 1H), 8.95 (s, broad, 1H), 10.2 (s, broad, 1H), 15.1 (s, broad, 1H).
  The singlet at 5.77 ppm corresponds to about one mol methylene dichloride per mol of substance (see Figure 13C).
  The XRD pattern of the product is shown in Figure 13A and the infrared spectrum obtained is shown in Figure 13B.
  The Moxifloxacine hydrochloride solvate with methylene dichloride is not hygroscopic (no water uptake after 1 day at 33% relative humidity.
Example 13.bMoxifloxacine hydrochloride anhydrous form IV
• [0101]
  2 g Moxifloxacine hydrochloride methylene dichloride solvate were dried in vacuum at 100°C for about 6 hours yielding 1,75 g of the desolvated anhydrous form IV of Moxifloxacine hydrochloride. The XRD pattern of the product is shown in Figure 14A and the infrared spectrum obtained is shown in Figure 14B.
Example 14preparation of Moxifloxacine hydrochloride solvate with acetic acidExample 14.a
• [0102]
  3,0 g (7,47 mmol) moxifloxacin were prepared according to EP 550903 and dissolved in 30 ml acetic acid at room temperature. To this solution 2,0 ml (2,1 eq) trimethylchlorosilane were added under stirring. 30 minutes after addition of the chlorosilane the crystallization started. The suspension was stirred for about 3,5 hours and the precipitate filtered off washed with acetonitrile and dried under vacuum at room temperature to yield 3,21g (86,3%) of the 1:1 solvate of Moxifloxacine hydrochloride with acetic acid.
  ¹H-NMR (DMSO-d6): 0.8 - 0.95 (m, 1H), 0.95 - 1.3 (m, 3H), 1.6 - 1.9 (m, 4 H), 1.9 (s, 3H), 2.55 - 2.75 (m, 1H), 2.8 - 3.0 (m, 1H), 3.1 - 3.25 (m, 1H), 3.5 - 3.7 (m with Singlet at 3.6 ppm, 4H), 3.7 - 3.8 (m, 1H), 3.8 - 4.0 (m, 2H), 4.0 - 4.2 (m, 2H), 7.63 (d, J = 14 Hz, 1H), 8.65 (s, 1H), 9.1 (s, broad, 1H), 10.4 (s, broad, 1H), 12.7 (s, broad, 1H).
  The singlet at 1.9 ppm corresponds to about one mol acetic acid per mol of substance (see Figure 15C).
  The XRD pattern of the product is shown in Figure 15A and the infrared spectrum obtained is shown in Figure 15B.
Example 14.b
• [0103]
  1,0 g (2,49 mmol) Moxifloxacin were prepared according to EP 550903 and dissolved in 5 ml acetic acid and 5 ml acetonitrile at room temperature. To this solution 0,38 ml (1,2 eq) trimethylchlorosilane were added under stirring.
  2 hours after addition of the chlorosilane the crystallization didn't start. To this solution 0,38 ml trimethylchlorosilane were once more added under stirring. The suspension was stored for about 17 hours at 4°C and the precipitate filtered off washed with acetonitrile and dried under vacuum at room temperature to yield 0,93g (75,0%) of the 1:1 solvate of Moxifloxacine hydrochloride with acetic acid.
Example 15preparation of Moxifloxacine hydrochloride solvate with nitromethane
• [0104]
  0,5 g (1,25 mmol) Moxifloxacin were prepared according to EP 550903 and dissolved in 15 ml nitromethane at appr. 60°C. To this solution 0,14 ml (2 eq) acetic acid and (2 eq) ml trimethylchlorosilane were added under stirring. The suspension was stored for about 17 hours and the precipitate was filtered off, washed with acetone and dried under vacuum at room temperature to yield 0,55g (88,2%) of the 1:1 solvate of Moxifloxacine hydrochloride with nitromethane.
  ¹H-NMR (DMSO-d6): 0.8 - 0.95 (m, 1H), 0.95 - 1.3 (m, 3H), 1.6 - 1.9 (m, 4 H), 2.55 - 2.75 (m, 1H), 2.8 - 3.0 (m, 1H), 3.1 - 3.25 (m, 1H), 3.5 - 3.7 (m with Singlet at 3.6 ppm, 4H), 3.7 - 3.8 (m, 1H), 3.8 - 3.95 (m, 2H), 4.0 - 4.2 (m, 2H), 4.44 (s, 3H), 7.63 (d, J = 14 Hz, 1H), 8.65 (s, 1H), 9.0 (s, broad, 1H), 10.3 (s, broad, 1H), 15.1 (s, broad, 1H).
  The singlet at 4.44 ppm corresponds to about one mol nitromethane per mol of substance (see Figure 16C).
  The XRD pattern of the product is shown in Figure 16A and the infrared spectrum obtained is shown in Figure 16B..............http://www.google.nl/patents/EP2145890B1?cl=en
  
   moxifloxacin synthesis
  
  syn.......http://newdrugapprovals.org/2014/02/19/moxifloxacin-bay-12-8039/
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  Puleʻanga Fakatuʻi ʻo Tonga

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  Tonga ([ˈtoŋa]; Tongan: Puleʻanga Fakatuʻi ʻo Tonga), officially the Kingdom of Tonga, is a Polynesian sovereign state and archipelago comprising 177 ...
  

  ‎Tupou VI - ‎Nuku'alofa - ‎Tongan - ‎His Majesty's Armed Forces

  You may not have heard of Tonga, but if you are an adventure buff, then you are definitely in for a treat. Tonga comprises 150 islands, 36 of which are inhabited and lived by people. These islands are very small, but offer very big in terms of tourism and leisure. Also, the guys love to try the customs of Tonga.
  Marriage Ceremonies
  To maximize the thrill of the experience, make sure you attend at least one marriage ceremony in Tonga. This should not be too hard as Tonga are very helpful and will be more than willing to invite into their ceremonies and festivities. Marriage ceremonies in Tonga are sensational and they love to attend one.
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  Tonga Customs
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  Although animals are not in abundance in Tonga, are nevertheless given prime importance. Flying foxes and iguanas are everywhere. You can even treat them as exotic foods, however, this practice is discouraged.
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  In Tonga, it is fun. And what's more fun than surfing in the Pacific? The tides in Tonga are perfect for this kind of water fun you should try, and you can try water skiing or canoeing water in these places like this will be fun for you and your family.
  Diving in Tonga
  Another fun water activities you can try in Tonga is scuba diving. Now, why is diving in Tonga much different than elsewhere? Just because Tonga is located at the bottom of the Pacific Ocean, the sea is abundant wildlife in which you may see water species rare and stunning coral formations through their own eyes.
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IR SPECTRUM OF IMPORTANT DRUGS

BRIEF DESCRIPTION OF THE DRAWINGS
• 
  
  
  
  • Figure 1B: Infrared spectrum of anhydrous Mycophenolate Mofetil hydrochloride.

  
   
  
  

  • Figure 2B: Infrared spectrum of Venlafaxine hydrochloride form I.

   
  
  
  

  • Figure 3B: Infrared spectrum of Venlafaxine hydrochloride form II.

   
  
  

  • Figure 4B: Infrared spectrum of Sertraline hydrochloride form II.

  
   
  
  

  • Figure 5B: Infrared spectrum of Sertraline hydrochloride form I.

   
  
  

  • Figure 6B: Infrared spectrum of Donepezil hydrochloride form II.

  
   
  

  • Figure 7B: Infrared spectrum of Donepezil hydrochloride form III.

   
  
  

  • Figure 8B: Infrared spectrum of Terbinafine hydrochloride form.

   
  
  

  • Figure 9B: Infrared spectrum of Cinacalcet hydrochloride.

  
   
  

  • Figure 10B: Infrared spectrum of Citalopram hydrobromide.

  
   
  

  • Figure 11 B: Infrared spectrum of Aripiprazole hydrochloride form A.

   
  
  

  • Figure 12B: Infrared spectrum of Pramipexole Monohydrochloride.

  
   
  

  • Figure 13B: Infrared spectrum of Moxifloxacin hydrochloride methylene dichloride solvate.

   
  
  

  • Figure 14B: Infrared spectrum of anhydrous Moxifloxacin hydrochloride form IV.

  
  
   
  
  
  
  
  
  
  
  

  • Figure 15B: Infrared spectrum of Moxifloxacin hydrochloride acetic acid solvate.

  
   
  

  • Figure 16B: Infrared spectrum of Moxifloxacin hydrochloride nitromethane solvate.

  
   
  
  

  • Figure 17B: Infrared spectrum of Duloxetine hydrochloride.

  
   
  
  

  • Figure 18B: Infrared spectrum of Linezolid hydrochloride.

  
   
  

  • Figure 19B: Infrared spectrum of Memantine hydrochloride.

  
   
  
  

  • Figure 20B: Infrared spectrum of Rimonabant Hydrochloride form I.

  
   
  

  • Figure 21 B: Infrared spectrum of Clopidogrel Hydrochloride form I.

  
   
  
  

  • Figure 22B: Infrared spectrum of Clopidogrel Hydrobromide form A.

  
   
  
  

  • Figure 23B: Infrared spectrum of Prasugrel Hydrochloride form B.

   
  
  

  • Figure 24B: Infrared spectrum of Prasugrel Hydrochloride acetonitrile solvate.

  
   
  

  • Figure 25B: Infrared spectrum of Raloxifene Hydrochloride form A.

   
  

  • .
  • Figure 26B: Infrared spectrum of Raloxifene Hydrochloride tetrahydrofurane solvate.
  •  
  •  
  •  
  • Figure 27B: Infr 
  • ared spectrum of Olanzapine Dihydrochloride form I.

  
  
   
  

  • Figure 28B: Infrared spectrum of Darifenacin Hydrobromide.
  • 
  • Figure 29B: Infrared spectrum of Sitagliptine Hydrochloride in amorphous form.

   
  

  • Figure 30B: Infrared spectrum of Vardenafil Dihydrochloride.

  
   
  
  

  • Figure 31 B: Infrared spectrum of Erlotinib Hydrochloride form A.

  
  

.

Deserts

Top Ten Largest Deserts in the World

The Karakum Desert, also spelled Kara Kum and Gara Gum is a desert  in Central Asia. It occupies about 70 percent, or 350,000 km², of the area of Turkmenistan. Covering much of present day Turkmenistan, the Karakum Desert lies east of the Caspian Sea, with the Aral Sea to the north and the Amu Darya river and the Kyzyl Kum desert to the northeast. In modern times, with the shrinking of the Aral Sea, the extended “Aral Karakum” has appeared on the former seabed, with an estimated area of 15,440 sq. The sands of the Aral Karakum are made up of a salt-marsh consisting of finely-dispersed evaporites and remnants of alkaline mineral deposits, washed into the basin from irrigated fields. The dusts blown on a powerful east-west airstream carry pesticide residues that have been found in the blood of penguins in Antarctica.10. Kara-Kum Desert, Uzbekistan / Turkmenistan

Lets read about top ten world’s largest deserts.

9. Great Sandy Desert, Australia

The Great Sandy Desert is a 360,000 km2 (140,000 sq mi) expanse in northwestern Australia. Roughly the same size as Japan, it forms part of a larger desert area known as the Western Desert. The vast region of Western Australia is sparsely populated, without significant settlements. The Great Sandy Desert is a flat area between the rocky ranges of the Pilbara  and the Kimberley. To the southeast is the Gibson Desert and to the east is the Tanami Desert. The Rudall River National Park and Lake Dora are located in the southwest while Lake Mackay is located in the southeast.

8. Chihuahuan Desert, Mexico

The Chihuahuan Desert is a desert that straddles the U.S.-Mexico border in the central and northern portions of the Mexican Plateau, bordered on the west by the extensive Sierra Madre Occidental range, and overlaying northern portions of the east range, the Sierra Madre Oriental. On the U.S.  side it occupies the valleys and basins of central and southern New Mexico, Texas  west of the Pecos River and southeastern Arizona; south of the border, it covers the northern half of the Mexican state of Chihuahua, most of Coahuila, north-east portion of Durango, extreme northern portion of Zacatecas  and small western portions of Nuevo León. It has an area of about 140,000 square miles. It is the third largest desert of the Western Hemisphere and is second largest in North America, after the Great Basin Desert.

7. Great Basin Desert, USA

The Great Basin is the largest watershed of North America which does not drain to an ocean. Water within the Great Basin evaporates since outward flow is blocked. The basin extends into Mexico and covers most of Nevada and over half of Utah, as well as parts of California, Idaho, Oregon and Wyoming. The majority of the watershed is in the North American Desert ecoregion, but includes areas of the Forested Mountain and Mediterranean California ecoregions. The Great Basin includes several metropolitan areas and Shoshone  Great Basin tribes. A wide variety of animals can be found in great basin desert. Look to the rocky slopes around the desert mountain ranges, you may spot a very rare desert bighorn sheep. Other mammals of the desert include kit fox, coyote, skunk, black-tailed jackrabbit, ground squirrels, kangaroo rat and many species of mice. Bird species are very diverse in desert oases.

6. Great Victoria Desert, Australia

The Great Victoria Desert is a barren, arid, and sparsely populated desert  ecoregion  in southern Australia. It falls inside the states of South Australia and Western Australia and consists of many small sandhills, grasslands  and salt lakes. It is over 700 kilometres (430 mi) wide (from west to east) and covers an area of 424,400 square kilometres (163,900 sq mi). The Western Australia Mallee shrub ecoregion lies to the west, the Little Sandy Desert to the northwest, the Gibson Desert and the Central Ranges xeric shrublands to the north, the Tirari  and Sturt Stony deserts to the east, and the Nullarbor Plain to the south separates it from the Southern Ocean.

Image credit: Travel  Collective

5. Patagonia Desert, Argentina

The Patagonian Desert, also known as the Patagonia Desert or the Patagonian Steppe, is the largest desert in America and is the 7th largest desert in the world by area, occupying 260,000 square miles (673,000 km). It is located primarily in Argentina with small parts in Chile and is bounded by the Andes, to its west, and the Atlantic Ocean to its east, in the region of Patagonia, southern Argentina. The Patagonian Desert is the largest continental landmass of the 40° parallel and is a large cold winter desert, where the temperature rarely exceeds 12°C and averages just 3°C. The region experiences about seven months of winter and five months of summer.

Image credit: Melissa  Toledo

4. Kalahari Desert, Southern Africa

The Kalahari Desert is a large arid to semi-arid sandy area in Southern Africa extending 900,000 square kilometers (350,000 sq), covering much of Botswana  and parts of Namibia and South Africa, as semi-desert, with huge tracts of excellent grazing after good rains. The Kalahari Desert is the southern part of Africa, and the geography is a portion of desert and a plateau. The Kalahari supports some animals and plants because most of it is not a true desert. There are small amounts of rainfall and the summer temperature is very high. It usually receives 3–7.5 inches (76–190 mm) of rain per year. The surrounding Kalahari Basin covers over 2,500,000 square kilometers (970,000 sq mi) extending farther into Botswana, Namibia and South Africa, and encroaching into parts of Angola, Zambia and Zimbabwe. The only permanent river, the Okavango, flows into a delta  in the northwest, forming marshes that are rich in wildlife.

Via: wikipedia

3. Gobi Desert, Mongolia / N.E China

The Gobi is a large desert  region in Asia. It covers parts of northern and northwestern China, and of southern Mongolia. The desert basins of the Gobi are bounded by the Altai Mountains and the grasslands and steppes of Mongolia on the north, by the Hexi Corridor and Tibetan Plateau to the southwest, and by the North China Plain to the southeast. The Gobi is made up of several distinct ecological and geographic regions based on variations in climate and topography. This desert is the fifth largest in the world. The Gobi is most notable in history as part of the great Mongol Empire, and as the location of several important cities along the Silk Road.

Image Credit: PnP

2. Arabian Desert, peninsula

Arabian Desert or Eastern Desert, c.86,000 sq mi (222,740 sq km), E Egypt, bordered by the Nile valley in the west and the Red Sea and the Gulf of Suez in the east. It extends along most of Egypt’s eastern border and merges into the Nubian Desert in the south. The Arabian Desert is sparsely populated; most of its inhabitants are based around wells and springs. Today most of the desert can be accessed by roads. Since ancient times Egypt has used the porphyry, granite, limestone, and sandstone found in the desert mountains as building materials. Oil is produced in the north. The name Arabian Desert is also commonly applied to the desert of the Arabian Peninsula.

Image Credit1.  Sahara Desert, North Africa

The Sahara is the world’s largest desert. At over 9,000,000 square kilometers (3,500,000 sq mi), it covers most of Northern Africa, making it almost as large as the United States or the continent of Europe. The desert stretches from the Red Sea, including parts of the Mediterranean coasts, to the outskirts of the Atlantic Ocean. To the south, it is delimited by the Sahel: a belt of semi-arid tropical savanna that comprises the northern region of central and western Sub-Saharan Africa.

Top Ten Largest Deserts in the World
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