Methyl cyanoacetate → 6,7-Dimethoxy-4-(3,4-dimethoxyphenyl)quinazoline-2-acetic acid methyl ester

HRID 266120노트

반응식

HRID 266120 반응식
[Cl-].[Al+3].[Cl-].[Cl-].[NH2:5][C:6]1[CH:23]=[C:22]([O:24][CH3:25])[C:21]([O:26][CH3:27])=[CH:20][C:7]=1[C:8]([C:10]1[CH:15]=[CH:14][C:13]([O:16][CH3:17])=[C:12]([O:18][CH3:19])[CH:11]=1)=O.[C:28]([CH2:30][C:31]([O:33][CH3:34])=[O:32])#[N:29]>O>[CH3:19][O:18][C:12]1[CH:11]=[C:10]([C:8]2[C:7]3[C:6](=[CH:23][C:22]([O:24][CH3:25])=[C:21]([O:26][CH3:27])[CH:20]=3)[N:5]=[C:28]([CH2:30][C:31]([O:33][CH3:34])=[O:32])[N:29]=2)[CH:15]=[CH:14][C:13]=1[O:16][CH3:17]

참가 물질

5

반응물 3

HCID 7747Methyl cyanoacetateHCID 6451240Aluminum(III) ChlorideHCID 99269672-Amino-4,5,3',4'-tetramethoxybenzophenone

생성물 1

HCID 212240726,7-Dimethoxy-4-(3,4-dimethoxyphenyl)quinazoline-2-acetic acid methyl ester

시약·촉매·용매 1

HCID 962Water용매

반응 조건

온도
100 °C

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.

후처리

  1. extractionextracted with chloroform
  2. washThe chloroform layer was washed with water
  3. dry with materialdried over magnesium sulfate
  4. washThe fractions eluted with hexane-ethyl acetate (4:1

출처 및 근거

ORD 기록
ord-41f7c6e978974dc5ae6e3a2c6dd0184f
출처 데이터셋
uspto-grants-1997_07
특허 번호
US05650410

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