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

Thursday, 3 September 2015

Tempone der with propargylamine




Example 23 Synthesis of Nitroxyl-Antiestrogen Hybrid 3-7
The syntheses of 3-2 proceeded according to Scheme 19.
Figure US20120046461A1-20120223-C00053
Tempone 3-1 (1.57 g, 9.22 mmol) and propargylamine (0.7 mL, 10.93 mmol) were dissolved in 1,2-dichloroethane (10 mL) to give a yellow solution. Acetic acid (0.67 mL, 10.95 mmols) was added causing an orange gelatinous precipitate. The reaction stirred under Argon for 24 h. Sodium triacetoxyborohydride (3.52 g, 16.6 mmol) was added neat and the reaction continued under Argon for 48 h after which the solvent was removed under reduced pressure leaving an orange oil. The oil was taken up in ethyl acetate (15 mL) and stirred at 40° C. for 1 h and then filtered. Florisil was added to the filtrate and the solvent removed under reduced pressure. Flash chromatography yielded 3-2 (1.542 g, 80%) as an orange solid.
Rf (ethyl acetate): 0.2
IR: 3400 cm−1, 3300 cm−1 and 3000 cm−1

m.p.: 65-67° C.
http://www.google.com/patents/US20120046461





 

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