Tetrahydrofuran → 4-Amino-2-[4-(2,4-hexadienoyl)-1-piperazinyl]-6,7-dimethoxyquinazoline

HRID 2295740

반응식

HRID 2295740 반응식
O1CCCC1.[NH2:6][C:7]1[C:16]2[C:11](=[CH:12][C:13]([O:19][CH3:20])=[C:14]([O:17][CH3:18])[CH:15]=2)[N:10]=[C:9]([N:21]2[CH2:26][CH2:25][NH:24][CH2:23][CH2:22]2)[N:8]=1.[C:27](Cl)(=[O:33])[CH:28]=[CH:29][CH:30]=[CH:31][CH3:32]>C(N(CC)CC)C>[NH2:6][C:7]1[C:16]2[C:11](=[CH:12][C:13]([O:19][CH3:20])=[C:14]([O:17][CH3:18])[CH:15]=2)[N:10]=[C:9]([N:21]2[CH2:26][CH2:25][N:24]([C:27](=[O:33])[CH:28]=[CH:29][CH:30]=[CH:31][CH3:32])[CH2:23][CH2:22]2)[N:8]=1

참가 물질

5

반응물 3

HCID 8028TetrahydrofuranHCID 5653802,4-Hexadienoyl chlorideHCID 6162672-(1-Piperazinyl)-4-amino-6,7-dimethoxyquinazoline

생성물 1

HCID 539144324-Amino-2-[4-(2,4-hexadienoyl)-1-piperazinyl]-6,7-dimethoxyquinazoline수율 85.1%

시약·촉매·용매 1

HCID 8471Triethylamine용매

실험 절차

To 20 ml of tetrahydrofuran were added 1.16 g of 4-amino-6,7-dimethoxy-2-(1-piperazinyl)quinazoline and 1.5 g of triethylamine. There was then added 0.52 g of 2,4-hexadienoyl chloride, after which the mixture was stirred at room temperature for 3 hours. The reaction mixture was then concentrated by evaporation under reduced pressure, and the resulting residue was washed with water and recrystallized from ethanol, to give 1.3 g of the desired Compound No. 10 in the form of pale yellow powdery crystals melting at 231°-233° C.

후처리

  1. concentrationThe reaction mixture was then concentrated by evaporation under reduced pressure
  2. washthe resulting residue was washed with water
  3. customrecrystallized from ethanol

출처 및 근거

ORD 기록
ord-d75f29afa8ca4004a106fdc9f25009b4
출처 데이터셋
uspto-grants-1984_01
특허 번호
US04426382

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