DR ANTHONY MELVIN CRASTO,WorldDrugTracker, helping millions, A 90 % paralysed man in action for you, I am suffering from transverse mylitis and bound to a wheel chair, With death on the horizon, nothing will not stop me except God................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

Saturday, 14 July 2018

National award to Anthony Melvin Crasto for contribution to Pharma society from Times Network for Excellence in HEALTHCARE) | 5th July, 2018 | Taj Lands End, Mumbai, India

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DR ANTHONY MEVIN CRASTO Conferred prestigious individual national award at function for contribution to Pharma society from Times Network, National Awards for Marketing Excellence ( For Excellence in HEALTHCARE) | 5th July, 2018 | Taj Lands End, Mumbai India

times now 5

TIMES NOW 2 TIMES NOW 3
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////////////National award,  contribution to Pharma society, Times Network, Excellence in HEALTHCARE,  5th July, 2018, Taj Lands End, Mumbai,  India, ANTHONY CRASTO
#hotpersoninawheelchair
#worlddrugtracker

Wednesday, 4 July 2018

SNS-Ligands for Ru-Catalyzed Homogeneous Hydrogenation and Dehydrogenation Reactions

Abstract Image
A detailed study of literature-known and novel S-containing pincer-type ligands for ruthenium-catalyzed homogeneous hydrogenation and dehydrogenation reactions was carried out. The scope and limitations of these catalysts were carefully investigated, and it was shown that simple bench-stable SNS–Ru complexes can be used to facilitate the hydrogenation of a variety of different substrates at a maximum H2 pressure of 20 bar under operationally simple, easy to scale up, glovebox-free conditions by using starting materials and reagents that do not require any special purification prior to use. It was also shown that such complexes can be used to catalyze the dehydrogenative coupling of alcohols and amines to get amides as well as for the dehydrogenative dimerization of alcohols to esters.

SNS-Ligands for Ru-Catalyzed Homogeneous Hydrogenation and Dehydrogenation Reactions

Institute of Organic ChemistryJohannes Kepler University LinzAltenbergerstr. 69, 4040 Linz, Austria
Patheon Austria, part of Thermo Fisher ScientificSt. Peterstr. 25, 4020 Linz, Austria
Org. Process Res. Dev., Article ASAP
DOI: 10.1021/acs.oprd.8b00142
*E-mail: mario.waser@jku.at. Tel: +4373224685411. Fax: +437322468545402., *E-mail: axel.zimmermann@patheon.com.
 
Complex IIb:
STR1
Method A was applied, using 180 mg of ligand 11b (1.09 mmol) and 993 mg of 27 (1.04 mmol) to give the complex IIb as yellow powder in 83% yield. The complex was isolated as mixture of three isomers.
 
1 H-NMR (CDCl3, 300 MHz, 298 K), δ / ppm: 7.75-7.50 (m, 10H), 7.41-7.25 (m, 16H), 5.05 (bs, 1H), 3.73-2.9 (m, 9H), 2.71-2.41 (m, 3H), 1.89-1.71 (m, 1H), 1.64-1.54 (m, 12H);
 
31P-NMR (CDCl3, 121 MHz, 298 K), δ / ppm: 50.6 (59%), 49.0 (24%), 47.6 (17%);
 
13C NMR (75 MHz, CDCl3, 298 K): δ / ppm = 137.1 (d, J = 39.5 Hz), 134.6 (d, J = 10.0 Hz), 129.3, 127.8 (d, J = 8.9 Hz), 49.0, 42.2, 17.7;
HRMS (ESI+): m/z calcd for C24H30ClNPRuS2 [M - Cl]+: 564.0284; found: 564.0272.
STR1
1 H-NMR (CDCl3, 300 MHz, 298 K), δ / ppm: 7.75-7.50 (m, 10H), 7.41-7.25 (m, 16H), 5.05 (bs, 1H), 3.73-2.9 (m, 9H), 2.71-2.41 (m, 3H), 1.89-1.71 (m, 1H), 1.64-1.54 (m, 12H);
STR2
31P-NMR (CDCl3, 121 MHz, 298 K), δ / ppm: 50.6 (59%), 49.0 (24%), 47.6 (17%);
str3
13C NMR (75 MHz, CDCl3, 298 K): δ / ppm = 137.1 (d, J = 39.5 Hz), 134.6 (d, J = 10.0 Hz), 129.3, 127.8 (d, J = 8.9 Hz), 49.0, 42.2, 17.7;
 
 
///////////////SNS-Ligands, Ru-Catalyzed,  Homogeneous Hydrogenation, Dehydrogenation Reactions

A borrowing hydrogen methodology: palladium-catalyzed dehydrative N-benzylation of 2-aminopyridines in water

Graphical abstract: A borrowing hydrogen methodology: palladium-catalyzed dehydrative N-benzylation of 2-aminopyridines in water

A borrowing hydrogen methodology: palladium-catalyzed dehydrative N-benzylation of 2-aminopyridines in water

 
 Author affiliations

Isao Azumaya

Abstract

We demonstrate a greener borrowing hydrogen methodology using the π-benzylpalladium system, which offers an efficient and environmentally friendly dehydrative N-monobenzylation of 2-aminopyridines with benzylic alcohols in the absence of base. The crossover experiment using benzyl-α,α-d2 alcohol and 3-methylbenzyl alcohol afforded H/D scrambled products, suggesting that the dehydrative N-benzylation in our catalytic system involves a borrowing hydrogen pathway. KIE experiments show that C–H bond cleavage at the benzylic position of benzyl alcohol is involved in the rate-determining step (KIE = 2.9). This simple base-free protocol can be achieved under mild conditions in an atom-economic process, affording the desired products in moderate to excellent yields.
N-Benzylpyridin-2-amine 3a 1 Yield 165 mg (90%) as a white solid; mp 90-91 C; IR (KBr) (cm-1) 3226, 3029, 1600, 1575; 1H NMR (400 MHz, CDCl3):  4.50 (d, J=5.7 Hz, 2H), 4.95 (brs, 1H), 6.36 (dt, J=8.5, 0.9 Hz, 1H), 6.58 (ddd, J=7.1, 5.0, 0.9 Hz, 1H), 7.23-7.36 (m, 4H), 7.39 (dd, J=8.7, 7.1, 1.8 Hz, 1H), 8.09 (ddd, J=5.0, 1.8, 0.9 Hz, 2H); 13C-NMR (100 MHz, CDCl3): 46.3, 106.8, 113.1, 127.2, 127.4, 128.6, 137.5, 139.2, 148.2, 158.6; MS (FAB): m/z 185 [M+H]+ .
STR2STR1
/////////////borrowing hydrogen methodology, palladium-catalyzed,  dehydrative N-benzylation, 2-aminopyridines,

Tuesday, 3 July 2018

CH4630808



CH4630808
syn   https://newdrugapprovals.org/2018/07/02/ch4630808/
Paper
Development of a Kilogram-Scale Synthesis of a Novel Anti-HCV Agent, CH4930808
CH4630808 corrected
 Research Division, Chugai Pharmaceutical Co., Ltd., 1-135 Komakado, Gotemba, Shizuoka 412-8513, Japan
 Pharmaceutical Technology Division, Chugai Pharmaceutical Co., Ltd., 5-5-1 Ukima, Kita-ku, Tokyo 115-8543, Japan
§ Department of Chemistry for Materials, Graduate School of Engineering, Mie University, Tsu, Mie 514-8507, Japan
Org. Process Res. Dev.201822 (2), pp 236–240
DOI: 10.1021/acs.oprd.7b00383
*E-mail: haneishitys@chugai-pharm.co.jp. Tel.: +81-550-87-9102. Fax: +81-550-87-5326.

Abstract

Abstract Image
Herein, we report the kilogram-scale synthesis of CH4930808 (1) CH 4630808 CORRECTED, a novel anti-hepatitis C virus agent. While pursuing improved productivity using many through-process strategies, we conducted scrupulous impurity control. Finally, we successfully developed a practical and scalable process for the synthesis of (1·1.5Na·2.5H2O), by which we prepared 3.28 kg of the active pharmaceutical ingredient for clinical studies
1H-NMR and 13C-NMR spectra of compound 5·HCl S 3– S 4
1H-NMR spectra of compound 1·1.5 Na·2.5 H2O S 5
13C-NMR spectra compound 1·1.5 Na·2.5 H2O S 6
1H-COSY spectra of compound 1·1.5 Na·2.5 H2O S 7 – S 8
DEPT spectra of compound 1·1.5 Na·2.5 H2O S 9 – S 10
HMBC spectra of compound 1·1.5 Na·2.5 H2O S 11 – S 17
MASS



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Saturday, 30 June 2018

Abiraterone Acetate



Abiraterone Acetate (1)
syn https://newdrugapprovals.org/2018/07/01/bms-986169/
1 in 81% yield (1.8 kg). HPLC Purity: 99.72%, Assay: 98.8% (HPLC, w/w). MS: m/z = 392.7 [M + H]+. IR (KBr) (cm–1): 3047, 2936, 1735, 1244, 1035, 801, 714. 1H NMR (400 MHz, DMSO-d6): δ 8.58 (s, 1 H), 8.43–8.42 (d, 1 H), 7.76–7.74 (d, 1 H), 7.34–7.31 (dd, 1 H), 6.11 (s, 1 H), 5.38 (s, 1 H), 4.44 (m, 1H), 2.19–2.50 (m, 3H), 1.98–2.08 (m, 6H), 1.39–1.85 (m, 9H), 1.03–1.11 (m, 8H). 13C NMR (CDCl3): δ 170.4, 151.6, 147.9, 147.8, 140.0, 133.6, 132.9, 129.1, 122.9, 122.2, 73.8, 57.4, 50.2, 47.3, 38.1, 36.9, 36.7, 35.1, 31.7, 31.4, 30.3, 27.7, 21.4, 20.8, 19.2, 16.5.
Abiraterone (2)
2 (2.88 kg, 72%) as a white solid. HPLC Purity: 99.87%. MS: m/z = 350.3 [M + H]+. IR (KBr) (cm–1): 3236, 3062, 3031, 2931,1596, 1065, 803. 1H NMR (400 MHz, CDCI3): δ 8.61 (s, 1 H), 8.44–8.46 (d, 1 H), 7.63–7.65 (d, 1 H), 7.20–7.23 (dd, 1 H), 5.993–5.996 (d, 1 H), 5.38–5.99 (d, 1 H), 3.48–3.54 (m, 1 H), 2.24–2.32 (m, 3H), 1.97–2.10 (m, 3H), 1.47–1.86 (m, 10H), 1.04–1.10 (s, 8H). 13C NMR (CDCl3): δ 16.58, 19.34, 20.88, 30.45, 31.52, 31.63, 31.81, 35.27, 36.71, 37.20, 42.32, 47.34, 50.37, 57.56, 71.62, 121.28, 123.03, 129.24, 132.99, 133.70, 141.21, 147.79, 147.88, 151.68
see supp info


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PAPER
Improved Procedure for Preparation of Abiraterone Acetate
Chemical Research Division, Ranbaxy Research Laboratory, Gurgaon, Haryana 122001, India
Org. Process Res. Dev.201418 (4), pp 555–558
DOI: 10.1021/op500044p
*E-mail: Mukesh.madhra@ranbaxy.com. Tel: (91-124)4011832.

Absolute Quantification of Lipophilic Shellfish Toxins by Quantitative Nuclear Magnetic Resonance Using Removable Internal Reference Substance with SI Traceability

Absolute Quantification of Lipophilic Shellfish Toxins by Quantitative Nuclear Magnetic Resonance Using Removable Internal Reference Substance with SI Traceability
Tsuyoshi KATO, Maki SAITO, Mika NAGAE, Kazuhiro FUJITA, Masatoshi WATAI, Tomoji IGARASHI, Takeshi YASUMOTO, and Minoru INAGAKI
Keywords: Lipophilic shellfish toxin, okadaic acid, dinophysistoxin-1, polyethers, qNMR, AQARI
Analytical Sciences2016, 32(7), 729.
DOI: 10.2116/analsci.32.729
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