Dichloromethane → 2-[2-(N,N-diethylamino)ethyl]-4-(3,4-dimethoxyphenyl)-6,7-dimethoxyquinazoline

HRID 1458943ノート

反応式

HRID 1458943 の反応式
Br[CH2:2][CH2:3][C:4]1[N:13]=[C:12]([C:14]2[CH:19]=[CH:18][C:17]([O:20][CH3:21])=[C:16]([O:22][CH3:23])[CH:15]=2)[C:11]2[C:6](=[CH:7][C:8]([O:26][CH3:27])=[C:9]([O:24][CH3:25])[CH:10]=2)[N:5]=1.[CH2:28]([NH:30][CH2:31][CH3:32])[CH3:29].ClCCl>O>[CH2:28]([N:30]([CH2:2][CH2:3][C:4]1[N:13]=[C:12]([C:14]2[CH:19]=[CH:18][C:17]([O:20][CH3:21])=[C:16]([O:22][CH3:23])[CH:15]=2)[C:11]2[C:6](=[CH:7][C:8]([O:26][CH3:27])=[C:9]([O:24][CH3:25])[CH:10]=2)[N:5]=1)[CH2:31][CH3:32])[CH3:29]

参加物

5

反応物 3

HCID 6344DichloromethaneHCID 8021DiethylamineHCID 220975842-(2-Bromoethyl)-4-(3,4-dimethoxyphenyl)-6,7-dimethoxyquinazoline

生成物 1

HCID 220976622-[2-(N,N-diethylamino)ethyl]-4-(3,4-dimethoxyphenyl)-6,7-dimethoxyquinazoline収率 8.4%

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

A mixture of 2-(2-bromoethyl)-4-(3,4-dimethoxyphenyl)-6,7-dimethoxyquinazoline (0.486 g), diethylamine (0.41 g) and dichloromethane (10 ml) was stirred under reflux for 6 hours. The reaction mixture was poured into water and extracted with dichloromethane. The dichloromethane layer was washed with water and dried over magnesium sulfate, and the solvent was evaporated. The residue was subjected to column chromatography on silica gel. The fractions eluted with chloroform-ethyl acetate (1/1, v/v) gave 2-[2-(N,N-diethylamino)ethyl]-4-(3,4-dimethoxyphenyl)-6,7-dimethoxyquinazoline (0.040 g, 8%) which was then recrystallized from ethyl acetate-hexane. Colorless prisms. mp. 164°-166° C.

後処理

  1. temperatureunder reflux for 6 hours
  2. extractionextracted with dichloromethane
  3. washThe dichloromethane layer was washed with water
  4. dry with materialdried over magnesium sulfate
  5. customthe solvent was evaporated
  6. washThe fractions eluted with chloroform-ethyl acetate (1/1

出典と根拠

ORDレコード
ord-7428576384904210ac958682fce66b5f
出典データセット
uspto-grants-1998_12
特許番号
US05852039

反応ノート

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