Trans-tert-Butyl-2-(4-methoxyphenyl)-cyclopropylcarbamate

 Trans-tert-Butyl-2-(4-methoxyphenyl)-cyclopropylcarbamate

DPPA (11 mls, 50.9 mmol) was added to a stirred mixture of the product from Preparation 78 (8.9 g, 46.3 mmol), triethylamine (10.1 mls, 72.7 mmol) and tert-BuOH (75 mls). The mixture was heated at 90° C. for 43 h. When cool, the tert-BuOH was removed by evaporation and the resulting oily residue treated with saturated K₂CO₃ (120 ml) and then extracted with EtOAc (2×100 mls). The combined organic extracts were then evaporated under reduced pressure to give a brown solid which was purified by column chromatography using DCM:MeOH (98:2) as eluant to provide the title product (5.8 g, 148%);

¹HNMR (400 MHz, CDCl₃) δ: 1.07-1.14 (m, 2H), 1.44 (s, 9H), 1.93-2.06 (m, 1H), 2.62-2.71 (m, 1H), 3.80 (s, 3H), 4.72-4.88 (m, 1H), 6.80 (d, 2H), 7.08 (d, 2H).












LATUR, MAHARASHTRA, INDIA

http://en.wikipedia.org/wiki/Latur

Latur लातूर Lattalur, Ratnapur
City
Latur Location in Maharashtra, India
Coordinates: 18.40°N 76.56°ECoordinates: 18.40°N 76.56°E
Country	India
State	Maharashtra
Region	Aurangabad Division
District	Latur
Settled	Possibly 7th century AD
Government
• Body	Latur Municipal Corporation
• Mayor	Akhtar Shaikh
Area[1]
• Total	117.78 km2(45.48 sq mi)
Area rank	89
Elevation	515 m (1,690 ft)
Population (2011)
• Total	382,754
• Rank	89th
• Density	3,200/km2(8,400/sq mi)
Demonym	Laturkar
Languages
• Official	Marathi
Time zone	IST (UTC+5:30)
PIN	413 512 413 531
Telephone code	91-2382
Vehicle registration	MH-24
Sex ratio	923.54 ♀/1000 ♂
Literacy	89.67
Distance from Mumbai	497 kilometres (309 mi) E (land)
Distance fromHyderabad	337 kilometres (209 mi) NW (land)
Distance fromAurangabad, Maharashtra	294 kilometres (183 mi) SE (land)
Climate	BSh (Köppen)
Precipitation	666 millimetres (26.2 in)
Avg. summer temperature	41 °C (106 °F)
Avg. winter temperature	13 °C (55 °F)
http://www.citypopulation.de/world/Agglomerations.html

his Is The Famous 'Ganj-Golai' As The Central Place Of The Latur City. There Are 16 Roads Connecting To This Place And Seperate Markets i.e. Jewellers ...




लातूर जिल्हयातील चित्र संग्रह

1. Colleges and Universities
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   Rajarshi Shahu College...

    

   

   Government Medical College...

    

   

   M. S. Bidve Engineering College...

    

   

   Mahatma Basweshwar College L...

    

   

   Dayanand Pharmacy College L...

LATUR AIRPORT

LATUR AIRPORT













2012 Navratri Mahotsav in Latur





SOS Children's Village Latur











Latur, India: Carnival Resort









Ausa Near Latur







Chakur near Latur



Vilasrao Deshmukh's ancestral home at Babhalgaon village in Latur. Machindra Amle

















UDGIR: Udgir is one of the most important towns of Latur district. Udgir has a great historical significance. It has witnessed the war between the Marathas ...







The city of Latur is located in India's welathiest state, Maharashtra. Together with many of the surrounding villages, Latur was all but destroyed in the 

Ethyl-2-(4-chlorophenyl)cyclopropanecarboxylate

Ethyl-2-(4-chlorophenyl)cyclopropanecarboxylate

A mixture of 4-chlorostyrene (10.1 ml, 96 mmol) and rhodium acetate dimer (1 g, 4.5 mmol) in toluene (50 ml) was heated to 85° C. before adding ethyl diazoacetate (11.3 mls, 94 mmol) over 30 mins and the whole then heated at 80° C. for a further 1 h before concentration in vacuo. The residue was then purified by column chromatography using 1:2 DCM:pentane as eluant to give the title product as a colourless oil (7.8 g, 37%); R_f 1:2 (DCM:pentane) 0.35; 

¹HNMR (400 MHz, CDCl₃) δ 1.15-1.3 (m, 4H), 1.5-1.7 (m, 1H), 1.8-1.9 (m, 1H), 2.4-3.55 (m, 1H), 4.2 (q, 2H), 6.95 (d, 2H), 7.20-7.28 (m, 2H); and LRMS: m/z, M+NH₄+242.

trans-2-(4-Chlorophenyl)cyclopropanecarboxylic acid

The product from preparation 73 (7.8 g, 37 mmol) was dissolved in EtOH (75 mls) at room temperature under nitrogen and sodium methoxide (8.1 g, 150 mmol) was added portionwise over 15 mins. After the addition was complete, the mixture was then refluxed for 18 h. The reaction mixture was concentrated in vacuo, and the resulting residue diluted with DCM and water (150 mls, 2:1 mixture). The organic layer was removed, and the aqueous layer re-extracted with DCM (2×50 mls). The combined organic extracts were dried over MgSO₄ and evaporated to provide the trans ester (4.96 g, 62%). Acidification of the aqueous layer with concentrated HCl to pH 1 resulted in a white precipitate, which was filtered and dried under vacuum to provide the hydrolysis product (the corresponding acid) as a white powder (1 .95 g, 27%). Dissolution of the ester in MeOH (50 mls), water (50 mls) and LiOH (1.34 g, 32 mmol) gave a clear solution which was heated at ca. 70° C. overnight. The reaction mixture was cooled, concentrated in vacuo, and acidified with concentrated HCl to pH 1. The resulting white precipitate was extracted with EtOAc (3×50 mls) and the combined organic extracts were dried over MgSO₄ and evaporated to dryness, to provide the acid (4 g, 96%). This acid was combined with the hydrolysed product from the previous step to give a total of 5.95 g; 

¹HNMR (400 MHz, CDCl₃) δ 1.3-1.4 (m, 1H), 1.6-1.7 (m, 1H), 1.8-1.9 (m, 1H), 2.5-2.6 (m, 1H), 7.00 (d, 2H), 7.26 (d, 2H); LRMS: m/z, M-H 195.

DRUG APPROVALS BY DR ANTHONY MELVIN CRASTO .....FOR BLOG HOME CLICK HERE Join me on Linkedin Join me on Facebook FACEBOOK Join me on twitter      Join me on google plus Googleplus  amcrasto@gmail.com KHAJURAHO , MADHYA PRADESH, INDIA Location of Khajuraho Group of Monuments in India. Location in Madhya Pradesh Khajuraho Group of Monuments - Wikipedia, the free ... en.wikipedia.org/wiki/Khajuraho_Group_of_Monuments The Khajuraho Group of Monuments are a group of Hindu and Jain temples in Madhya Pradesh, India. About 620 kilometres (385 mi) southeast of New Delhi, ... Hotel Chandela - A Taj Leisure Hotel

tert-Butyl 2-(2-acetylhydrazino)-2-oxoethylcarbamate

 tert-Butyl 2-(2-acetylhydrazino)-2-oxoethylcarbamate

2-Ethoxy-1-ethoxycarbonyl-1,2-dihydroquinoline (7.06 g, 28.5 mmol) was added to a solution of N-tert-butoxycarbonylglycine (5.0 g, 28.6 mmol) in dichloromethane (75 ml), and the solution stirred for 15 minutes. Acetic hydrazide (2.6 g, 35.1 mmol) was added, and the reaction stirred at room temperature for 18 hours. The resulting precipitate was filtered, and dried in vacuo, to afford a white crystalline solid, 2.42 g. The filtrate was concentrated under reduced pressure, diluted with ether, and the resulting precipitate filtered and dried in vacuo, to afford additional product as a white solid, 4.4 g, 67% in total; 

¹H NMR (CDCl₃, 400 MHz) δ: 1.41 (s, 9H), 2.02 (s, 3H), 3.87 (d, 2H), 5.22 (bs, 1H), 8.27 (bs, 1H), 8.84 (bs, 1H); LRMS: m/z 249.2 (MNH₄ ⁺);

2-[2-(2-Oxo-1-piperidinyl)ethyl]-1H-isoindole-1,3(2H)-dione

2-[2-(2-Oxo-1-piperidinyl)ethyl]-1H-isoindole-1,3(2H)-dione

Pthalimide (952 mg, 6.47 mmol) was added to a solution of the product from preparation 5 (842 mg, 5.88 mmol) in tetrahydrofuran (30 ml), and the mixture sonicated until a solution was obtained. Polymer supported triphenyl phosphine (2.5 g, 7.5 mmol) and diethyl azodicarboxylate (1.15 ml, 7.31 mmol) were added, and the reaction stirred at room temperature for 18 hours. The mixture was filtered through Arbocel®, the filtrate concentrated under reduced pressure and the residue azeotroped with dichloromethane. The crude product was purified by column chromatography on silica gel using an elution gradient of ethyl acetate:pentane (70:30 to 100:0), to give the title compound as a white foam, 1.6 g (containing some impurities); 

¹H NMR (CDCl₃, 400 MHz) δ: 1.60-1.80 (m, 4H), 2.17 (m, 2H), 3.30 (m, 2H), 3.60 (m, 2H), 3.83 (m, 2H), 7.62 (m, 2H), 7.79 (m, 2H); LRMS: m/z 273.2 (MH⁺).

tert-Butyl-3-bromopropionate

tert-Butyl-3-bromopropionate

To a solution of 3-bromopropionic acid (6.0 kg, 39.2 mol) in dichloromethane (60 L) at 0° C. was added tert-butanol (0.6 L) and conc. sulfuric acid (0.33 L). The resultant solution was cooled to −15° C. and isobutylene was bubbled through (11 kg, 196 mol). The reaction was then stirred for 3 hours at −5° C. before warming to 20° C. over 4 hours and was then stirred at this temperature for 15 hours. The reaction was quenched by cautious addition into saturated aqueous sodium bicarbonate solution (0.6 M, 72 L, 43.2 mol). The layers were then separated and the organic layer was washed with saturated aqueous sodium bicarbonate solution (2×48 L) followed by deionised water (48 L). This washing cycle was repeated and the pH of the aqueous layer was measured and was shown to be above pH 7. Potassium carbonate (90 g, 1.5% w/w) was added to the organic layer before concentrating the solution to a volume of 9 L by distillation at atmospheric pressure. Tetrahydrofuran (40 L) was added and the remainder of the dichloromethane was removed by distillation at atmospheric pressure to give a solution (12 L) of the title compound (5.27 kg, 25.2 mol, 64% yield) in tetrahydrofuran that was used directly in the next step;

¹H-NMR (CDCl₃, 300 MHz,) δ: 1.45 (s, 9H), 2.80 (t, 2H), 3.53 (t, 2H); LRMS (El): m/z [MH⁺] 209 (⁷⁹Br).

EASY NMR

 Benzyl 2-{[1-(chlorocarbonyl)cyclopentyl]methyl}entanoate

Oxalyl chloride (1.15 ml, 13.2 mmol) was added to an ice-cooled solution of 1-{2-[(benzyloxy)carbonyl]pentyl}cyclopentanecarboxylic acid (EP 274234, Example 16) (2.0 g, 6.3 mmol) in dry dichloromethane (20 ml), and the solution stirred at room temperature for 2 hours. The reaction mixture was concentrated under reduced pressure and the residue azeotroped with dichloromethane (3×), to give the title compound as a golden oil, 2.1 g; 

¹H NMR (CDCl₃, 300 MHz) δ: 0.88 (t, 3H), 1.28 (m, 2H), 1.43 (m, 2H), 1.63 (m, 6H), 2.00 (m, 1H), 2.08-2.35 (m, 3H), 2.44 (m, 1H), 5.15 (s, 2H), 7.28 (m, 5H).

N-Methoxy-N-methyl-2-(2-oxo-1-pyrrolidinyl)acetamide

N-Methoxy-N-methyl-2-(2-oxo-1-pyrrolidinyl)acetamide

2-Chloro-N-methoxy-N-methylacetamide (ex Aldrich Chemical Co.) (3.2 g, 23.3 mmol) was added to a suspension of 2-pyrrolidinone (2.0 g, 23.5 mmol) and sodium hydride (940 mg, 60% dispersion in mineral oil, 23.5 mmol) in tetrahydrofuran (60 ml), and the reaction stirred at room temperature for 48 hours. The mixture was quenched with water (150 ml), and extracted with ethyl acetate (200 ml) and dichloromethane (200 ml). The combined organic extracts were dried (MgSO₄) and evaporated under reduced pressure. The residue was triturated with hexane, then ether to afford the title compound as white crystals, 1.8 g, 41%; 

¹H NMR (CDCl₃, 400 MHz) δ: 2.02 (m, 2H), 2.40 (t, 2H), 3.17 (s, 3H), 3.48 (t, 2H), 3.72 (s, 3H), 4.19 (s, 2H); LRMS: m/z 186.9 (MH⁺).