반응 #353302

ord-41f7c6e978974dc5ae6e3a2c6dd0184f

용매

반응 조건

온도
100°CELSIUS
상세 조건
See reaction.notes.procedure_details.

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 hexane-ethyl acetate (4:1

실험 절차

Aluminium chloride powder (5.3 g) was added to a mixture of 2-amino-4,5,3',4'-tetramethoxybenzophenone (6.3 g) and methyl cyanoacetate (23 ml), and the mixture was stirred at 100° C. for 2.5 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 hexane-ethyl acetate (4:1, v/v) gave methyl 4-(3,4-dimethoxyphenyl)-6,7-dimethoxyquinazoline-2-acetate. This compound was recrystallized from acetone. Colorless needles, mp. 152°-153° C.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US05650410uspto-grants-1997_07