2-Mercaptoethanol → 6,7-Dimethoxy-4-(3,4-dimethoxyphenyl)-2-(2-hydroxyethylthiomethyl)quinazoline

HRID 617222ノート

反応式

HRID 617222 の反応式
Cl[CH2:2][C:3]1[N:12]=[C:11]([C:13]2[CH:18]=[CH:17][C:16]([O:19][CH3:20])=[C:15]([O:21][CH3:22])[CH:14]=2)[C:10]2[C:5](=[CH:6][C:7]([O:25][CH3:26])=[C:8]([O:23][CH3:24])[CH:9]=2)[N:4]=1.[SH:27][CH2:28][CH2:29][OH:30].C(=O)([O-])[O-].[K+].[K+].CN(C)C=O>O>[CH3:24][O:23][C:8]1[CH:9]=[C:10]2[C:5](=[CH:6][C:7]=1[O:25][CH3:26])[N:4]=[C:3]([CH2:2][S:27][CH2:28][CH2:29][OH:30])[N:12]=[C:11]2[C:13]1[CH:18]=[CH:17][C:16]([O:19][CH3:20])=[C:15]([O:21][CH3:22])[CH:14]=1

参加物

6

反応物 4

HCID 15672-MercaptoethanolHCID 6228DimethylformamideHCID 11430Potassium CarbonateHCID 107856562-Chloromethyl-4-(3,4-dimethoxyphenyl)-6,7-dimethoxyquinazoline

生成物 1

HCID 218511326,7-Dimethoxy-4-(3,4-dimethoxyphenyl)-2-(2-hydroxyethylthiomethyl)quinazoline収率 82%

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

A mixture of 2-chloromethyl-6,7-dimethoxy-4-(3,4-dimethoxyphenyl)quinazoline (4.5 9), 2-mercaptoethanol (1.13 g), potassium carbonate (2.8 9) and N,N-dimethylformamide (50 ml) was stirred at room temperature for 2 hours. The reaction mixture was poured into water and extracted with ethyl acetate. The ethyl acetate layer was washed with water and dried (MgSO4). The solvent was distilled off to obtain 6,7-dimethoxy-4-(3,4-dimethoxyphenyl)-2-[(2-hydroxyethylthio)methyl]quinazoline (4.1 g, 82%), and it was recrystallized from ethanol.

後処理

  1. extractionextracted with ethyl acetate
  2. washThe ethyl acetate layer was washed with water
  3. dry with materialdried (MgSO4)
  4. distillationThe solvent was distilled off

出典と根拠

ORDレコード
ord-df758846c27f42c0aa32624e1ca5b17b
出典データセット
uspto-grants-1999_09
特許番号
US05948782

反応ノート

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