반응 #353301

반응 방정식

Aluminium chloride

2-amino-4,5,3',4'-tetramethoxybenzophenone

chloroacetonitrile

→

2-chloromethyl-4-(3,4-dimethoxyphenyl)-6,7-dimethoxyquinazoline

수율 52.0%

용매

water

반응 조건

후처리

1. 1
   추출extracted with chloroform
2. 2
   세척The chloroform layer was washed with water
3. 3
   건조dried over magnesium sulfate
4. 4
   세척The fractions eluted with chloroform-ethyl acetate (10:1

실험 절차

Aluminium chloride powder (6.7 g) was added to a mixture of 2-amino-4,5,3',4'-tetramethoxybenzophenone (8.0 g) and chloroacetonitrile (25 ml), and the mixture was stirred at 100° C. for 2 hours. The reaction mixture was poured into water and extracted with chloroform. The chloroform layer was washed with water and dried over magnesium sulfate. The residue was subjected to column chromatography on silica gel. The fractions eluted with chloroform-ethyl acetate (10:1, v/v) gave 2-chloromethyl-4-(3,4-dimethoxyphenyl)-6,7-dimethoxyquinazoline (4.9 g, 52%). This compound was recrystallized from acetone. Colorless prisms, mp. 183°-184° C.

출처