Welcome to chemicalbook!
Chinese English Japanese Germany Korea
400-158-6606
Try our best to find the right business for you.
Do not miss inquiry messages Please log in to view all inquiry messages.

Welcome back!

216686-60-1

CHEMBRDG-BB 3000759 synthesis

2synthesis methods
-

Yield:216686-60-1 53%

Reaction Conditions:

with morpholine;sulfur in ethanol at 120; for 0.333333 h;Microwave irradiation;Gewald Aminoheterocycles Synthesis;

Steps:

General procedure for the synthesis of ortho amino esters (Gewald reaction) [3, 4].

General procedure: A mixtureof the respective aldehyde or ketone (1 eq), ethylcyanoacetate (1 eq), S8 (1.1 eq), and morpholine(1.5 eq) in EtOH (5 mL) was irradiated at 120 °C for 20 min under microwave conditions. Thereaction mixture was cooled and the solution was poured onto 20 mL ice water to yield a precipitatewhich was filtered, washed with water and dried under vacuum. The crude solid was recrystallizedfrom ethanol to yield the desired product. If the solid was not precipitated from water, extract theaqueous solution with EtOAc (2 x 15 mL) and the organic solution was washed with brine, driedover sodium sulfate and filtered. The solvent was evaporated in vacuo and recrystallized fromappropriate solvent.

References:

Kankanala, Jayakanth;Kirby, Karen A.;Huber, Andrew D.;Casey, Mary C.;Wilson, Daniel J.;Sarafianos, Stefan G.;Wang, Zhengqiang [European Journal of Medicinal Chemistry,2017,vol. 141,p. 149 - 161] Location in patent:supporting information