Diethyl Ether → Prazosin

HRID 461336노트

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HRID 461336 반응식
[C:1]([N:6]1[CH2:11][CH2:10][N:9]([C:12]2[N:21]=[C:20]([NH2:22])[C:19]3[C:14](=[CH:15][C:16]([O:25][CH3:26])=[C:17]([O:23][CH3:24])[CH:18]=3)[N:13]=2)[CH2:8][CH2:7]1)(OCC)=[O:2].[CH2:27]([O:29][CH2:30][CH3:31])[CH3:28]>>[O:29]1[CH:30]=[CH:31][CH:28]=[C:27]1[C:1]([N:6]1[CH2:7][CH2:8][N:9]([C:12]2[N:21]=[C:20]([NH2:22])[C:19]3[C:14](=[CH:15][C:16]([O:25][CH3:26])=[C:17]([O:23][CH3:24])[CH:18]=3)[N:13]=2)[CH2:10][CH2:11]1)=[O:2]

참가 물질

3

반응물 2

HCID 3283Diethyl EtherHCID 133706732-(4-Carbethoxypiperazin-1-yl)-4-amino-6,7-dimethoxyquinazoline

생성물 1

HCID 4893Prazosin

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온도
-20 °C

실험 절차

To the above mixture is added slowly at -20° C., 32.9 g. (0.10 mole) of 2-(4-carbethoxypiperazin-1-yl)-4-amino-6,7-dimethoxyquinazoline dissolved in 300 ml. of ethyl ether. The reaction mixture is stirred at -20° C. for 2 hours, then allowed to warm to room temperature. The resulting mixture is hydrolyzed by addition of 100 ml. of water, and the ether layer separated. The aqueous layer is extracted with 300 ml. of ether and the combined extracts are dried over anhydrous magnesium sulfate. Evaporation of solvent affords 2-[4-(2-furoyl)piperazin-1-yl]-4-amino-6,7-dimethoxyquinazoline which can be further pruified if desired by silica gel column chromatography.

후처리

  1. additionTo the above mixture is added slowly at -20° C.
  2. temperatureto warm to room temperature
  3. additionThe resulting mixture is hydrolyzed by addition of 100 ml
  4. customof water, and the ether layer separated
  5. extractionThe aqueous layer is extracted with 300 ml
  6. dry with materialof ether and the combined extracts are dried over anhydrous magnesium sulfate
  7. customEvaporation of solvent

출처 및 근거

ORD 기록
ord-84e6ad6aa6d945eca003f793f969127e
출처 데이터셋
uspto-grants-1977_12
특허 번호
US04062844

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