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

HRID 266140노트

반응식

HRID 266140 반응식
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]

참가 물질

5

반응물 3

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

생성물 1

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

시약·촉매·용매 1

HCID 962Water용매

실험 절차

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%). This compound was recrystallized from ethyl acetate - hexane. Colorless prisms, mp. 164°-166° C.

후처리

  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

출처 및 근거

ORD 기록
ord-028d32714d9946898980632e446eb078
출처 데이터셋
uspto-grants-1997_07
특허 번호
US05650410

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