반응 #576064

반응 방정식

hydrochloric acid

ethyl (2E)-3-[3-[7-chloro-3-(2-[[4-chloro-2-(trifluoromethyl)phenyl]amino]-2-oxoethyl)-6-methyl-2-oxo-2H-chromen-4-yl]phenyl]-2-propenoate

sodium hydroxide

→

title compound

수율 71.8%

(2E)-3-[3-[7-chloro-3-(2-[[4-chloro-2-(trifluoromethyl)phenyl]amino]-2-oxoethyl)-6-methyl-2-oxo-2H-chromen-4-yl]phenyl]-2-propenoic acid

수율 71.8%

용매

ethanol

THF

반응 조건

후처리

1. 1
   추출the mixture was extracted with ethyl acetate
2. 2
   세척The extract was washed with water
3. 3
   건조dried over magnesium sulfate
4. 4
   농축concentrated
5. 5
   기타The resultant crude crystal was recrystallized from THF-ethyl acetate

실험 절차

A solution of ethyl (2E)-3-[3-[7-chloro-3-(2-[[4-chloro-2-(trifluoromethyl)phenyl]amino]-2-oxoethyl)-6-methyl-2-oxo-2H-chromen-4-yl]phenyl]-2-propenoate (200 mg) in a mixture of ethanol (5 ml) and THF (2 ml) was combined with a 1 N aqueous solution of sodium hydroxide (3 ml), and stirred at room temperature for 4 hours. After 1 N hydrochloric acid (10 ml) was added, the mixture was extracted with ethyl acetate. The extract was washed with water, dried over magnesium sulfate, and then concentrated. The resultant crude crystal was recrystallized from THF-ethyl acetate to obtain the title compound as a colorless crystal (137 mg, yield: 70%). Melting point: 191-194° C.

출처