................DR ANTHONY MELVIN CRASTO Ph.D ( ICT, Mumbai) , INDIA 25Yrs Exp. in the feld of Organic Chemistry,Working for GLENMARK GENERICS at Navi Mumbai, INDIA. Serving chemists around the world. Helping them with websites on Chemistry.Million hits on google, world acclamation from industry, academia, drug authorities for websites, blogs and educational contribution
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Thursday, 16 November 2017
13 C NMR PREDICT
NMR IS EASY
MOM CAN TEACH
1 H NMR (600 MHz, CDCl3) δ 8.23 (s, 1H), 7.83 (d, J = 8.3 Hz, 1H), 7.71 (s, 1H) 7.44 (d, J = 7.6 Hz, 1H), 4.00–3.25 (br, 8H).
13C NMR (150 MHz, CDCl3) δ 169.52, 153.87, 149.67, 141.24, 132.90, 123.79, 120.76, 110.48, 66.81.
HRMS (DART) m/z calcd for C12H13N2O3 [MH]+ : 233.0926, found 233.0926.
4-(6-Benzoxazoyl)morpholine (8) ( 13C NMR, 150 MHz, CDCl3)
4-(6-Benzoxazoyl)morpholine (8) ( 1 H NMR, 600 MHz, CDCl3)
Tuesday, 14 November 2017
NMR IS EASY
MOM CAN TEACH
13C NMR PREDICT
“ORG SPECT INT” CATERS TO EDUCATION GLOBALLY, No commercial exploits are done or advertisements added by me. This is a compilation for educational purposes only. P.S. : The views expressed are my personal and in no-way suggest the views of the professional body or the company that I represent/////////////
Monday, 13 November 2017
NMR IS EASY
MOM CAN TEACH
13C NMR PREDICT
“ORG SPECT INT” CATERS TO EDUCATION GLOBALLY, No commercial exploits are done or advertisements added by me. This is a compilation for educational purposes only. P.S. : The views expressed are my personal and in no-way suggest the views of the professional body or the company that I represent
Friday, 10 November 2017
The synthesis of monocyclic, spirocyclic and fused bicyclic secondary amines bearing a gem-difluorocyclopropane moiety via difluorocyclopropanation of unsaturated N-Boc derivatives using the trifluoromethyl(trimethyl)silane/sodium iodide [CF3SiMe3-NaI] system is described. The relative order of the substrate reactivity is established. It is shown that for the reactive alkenes the standard reaction conditions can be used, whereas for the substrates with low reactivity, slow addition of the Ruppert–Prakash reagent is necessary.
Authors., Pavel S. Nosik,
DOI: 10.1002/adsc.201700857Pavel S. Nosik,a.b Andrii O. Gerasov,a Rodion O. Boiko,a Eduard Rusanov,b Sergey V. Ryabukhin,c Oleksandr O. Grygorenko,c * Dmitriy M. Volochnyukb
a Spectrum Info Ltd., Life Chemicals Inc., Murmanska Street 5, Kyiv 02094, Ukraine
b Institute of Organic Chemistry, National Academy of Sciences of Ukraine, Murmanska Street 5, Kyiv 02660, Ukraine
c National Taras Shevchenko University of Kyiv, Volodymyrska Street 64, Kyiv 01601, Ukraine
* Corresponding author. E-mail: firstname.lastname@example.org.
National Taras Shevchenko University of Kyiv, Volodymyrska Street 64, Kyiv 01601, Ukraine
Dmitriy M. Volochnyuk
Institute of Organic Chemistry, National Academy of Sciences of Ukraine, Murmanska Street 5, Kyiv 02660, Ukraine
Dmitriy M. Volochnyuk was born in 1980 in Irpen, Kyiv region, Ukraine. He graduated from Kyiv State Taras Shevchenko University in 2002 and was awarded his M.S. degree in chemistry. He received his Ph.D. in organic chemistry in 2005 from the Institute of Organic Chemistry, National Academy of Sciences of Ukraine under the supervision of Dr. A. Kostyuk for research on the chemistry of enamines. At present, he divides his time between the Institute of Organic Chemisty, as Deputy Head of Organophosphorus Department and Senior Researcher, and Enamine Ltd (Kyiv, Ukraine), as Director of Chemistry. His main scientific interests are related to fluoroorganic, organophosphorus, heterocyclic and combinatorial chemistry, and multistep organic synthesis. He is a coauthor of more than 80 papers
- Given that the incorporation of small fluorinated fragments in drug-like molecules continues to rise, this has created an onus on the synthetic community to provide robust, scalable routes to these molecules of interest. Grygorenko and co-workers have reported on a synthesis of amines featuring a gem-difluorocyclopropane moiety using the readily available Ruppert–Prakash reagent ( Adv. Synth. Catal. 2017, 10.1002/adsc.201700857).
- Evaluating a series of olefins under the standard reaction conditions in refluxing THF indicated that only the most reactive olefins (gem-disubstituted) provided good yields of the desired cyclopropane, while other solvents proved to be ineffective. Conducting a control experiment omitting the substrate demonstrated that the key issue herein was competitive decomposition of the TMSCF3 to a series of gaseous byproducts under the reaction conditions.
- Whereas continuous flow provides a potential to mitigate against this, the current report demonstrated that slow addition of the reagent to the reaction mixture also provided a practical solution to this problem.
- Employing this approach enabled not only excellent conversions and yields to be realized but also allowed reactivity trends to be identified. In general, gem-disubstituted are the most reactive with the trend correlating with steric hindrance.
- For other classes of olefins, electronics are the major factor with the ability of the substituents to stabilize a positive charge in the transition state consistent with a nonsynchronous formation of the two sigma bonds in the cycloaddition the key consideration. The removal of the Boc-protecting group under standard acidic conditions provided the amines as their hydrochloride salts.
- PhDHead of Crystallographic Lab./Director of the crystallographic facility Nat. Acad. of Sci. Ukraine 'Single Mjlecule Crystallography' at IOCInstitute of Organic Chemistry... · DEPARTMENT OF PHYSICOCHEMICAL INVESTIGATIONS
tert-Butyl 1,1-difluoro-6-azaspiro[2.5]octane-6-carboxylate (10a):
Yield: 66.7 g (91%) (Method A); off-white crystalline powder: mp 46–48 8C;
1H NMR (CDCl3 , 400 MHz): d= 3.57–3.42 (m, 2H), 3.40–3.27 (m, 2H), 1.66–1.47 (m, 4H), 1.44 (s, J=2.3 Hz, 9H), 1.08 (t, J=8.3 Hz, 2H);
13C NMR (CDCl3, 101 MHz): d=154.2, 115.4 (t, J=288.1 Hz), 79.3, 42.8, 28.4, 28.1, 26.8 (t, J=10.0 Hz), 21.0 (t, J=10.1 Hz);
19F NMR (CDCl3 , 376 MHz): email@example.com;
MS (EI): m/z= 247 (M+ ), 192 (M+@t-Bu), 174 (M+@t-BuO), 147 (M+@Boc), 127 (M+@Boc@HF);
Anal. calcd. for C12H19F2NO2 : C 58.29, H 7.74, N 5.66; found: C 58.49, H 8.02, N 5.30.
Thursday, 9 November 2017
Molecular Formula, C14H15N
Molecular Weight, 197.28
CAS Number, 1137-79-7
(1) N,N-dimethyl-[1,1'-biphenyl]-4-amine (3a) 5,6
Elute: EtOAc/petroleum ether: 1/100 (v/v), white solid, yield 97.8 mg (99%).
1H NMR (400 MHz, CDCl3): δ 7.56 (d, J = 7.8 Hz, 2H), 7.51 (d, J = 8.8 Hz, 2H), 7.40 (t, J = 7.7 Hz, 2H), 7.30–7.21 (m, 1H), 6.81 (d, J = 8.8 Hz, 2H), 3.00 (s, 6H).
13C NMR (101 MHz, CDCl3): δ 150.09, 141.34, 129.37, 128.78, 127.84, 126.43, 126.12, 112.90, 40.97.
5 Yang, X.; Wang, Z.-X. Organometallics 2014, 33, 5863.
(6) Stibingerova, I.; Voltrova, S.; Kocova, S.; Lindale, M.; Srogl, J. Org. Lett. 2016, 18, 312.
Transition-Metal-Free Cross-Coupling of Aryl and Heteroaryl Thiols with Arylzinc Reagents
† CAS Key Laboratory of Soft Matter Chemistry, Hefei National Laboratory for Physical Sciences at Microscale and Department of Chemistry, University of Science and Technology of China, Hefei, Anhui 230026, P. R. China
‡ Collaborative Innovation Center of Chemical Science and Engineering (Tianjin), Tianjin 300072, P. R. China
Org. Lett., Article ASAP
Cross-coupling of (hetero)arylthiols with arylzinc reagents via C–S cleavage was performed under transition-metal-free conditions. The reaction displays a wide scope of substrates and high functional-group tolerance. Electron-rich and -deficient (hetero)arylthiols and arylzinc reagents can be employed in this transformation. Mg2+ and Li+ ions were demonstrated to facilitate the reaction.
In summary, we developed a transition-metal-free coupling reaction of (hetero)arylthiols with arylzinc reagents to form bi(hetero)aryls. The reaction exhibited wide substrate scope and good compatibility of functional groups. Electron-rich and -poor aryl or heteroaryl thiols can be converted. Various arylzinc reagents, including electron-rich and electron-poor reagents, can be employed as the coupling partners. Preliminary mechanistic studies suggest a nucleophilic aromatic substitution pathway, and Mg2+ and Li+ ions play important roles in the process of reaction. This study provides an example of S2– as a leaving group in an aromatic system and an effective methodology for the synthesis of bi(hetero)aryls including pharmaceutical molecules without transition-metal impurities.
Zhong-Xia Wang is a professor in the Department of Chemistry at the University of Science and Technology of China. He received his BS degree (1983) and MS degree (1986) from Nankai University, and PhD degree (1997) from the University of Sussex, UK. Since July 1986, Wang has been working at the University of Science and Technology of China (USTC) successively as Assistant, Lecturer, Associate Professor, and Professor. From Aug. 1993 to Oct. 1996, he pursued his doctoral studies at the University of Sussex, UK, and from Oct. 1999 to Oct. 2000, he was a Research Associate at the Chinese University of Hong Kong. 学 系 Department of Chemistry Predicts