Ethanol → HCID 178457032, 화합물

HRID 1457484노트

반응식

HRID 1457484 반응식
C(O)C.[OH-].[K+].[C:6]1([CH2:12][CH2:13][N:14]2[C:18]([Br:19])=[C:17]([C:20]([O:22]CC)=[O:21])[C:16]([N:25]([CH2:44][CH2:45][CH3:46])[CH2:26][C:27]3[CH:32]=[CH:31][C:30]([C:33]4[CH:38]=[CH:37][CH:36]=[CH:35][C:34]=4[C:39]4[NH:43][N:42]=[N:41][N:40]=4)=[CH:29][CH:28]=3)=[N:15]2)[CH:11]=[CH:10][CH:9]=[CH:8][CH:7]=1>O>[C:6]1([CH2:12][CH2:13][N:14]2[C:18]([Br:19])=[C:17]([C:20]([OH:22])=[O:21])[C:16]([N:25]([CH2:44][CH2:45][CH3:46])[CH2:26][C:27]3[CH:32]=[CH:31][C:30]([C:33]4[CH:38]=[CH:37][CH:36]=[CH:35][C:34]=4[C:39]4[NH:43][N:42]=[N:41][N:40]=4)=[CH:29][CH:28]=3)=[N:15]2)[CH:11]=[CH:10][CH:9]=[CH:8][CH:7]=1

참가 물질

5

반응물 3

HCID 702EthanolHCID 14797Potassium HydroxideHCID 178457033HCID 178457033, 화합물

생성물 1

HCID 178457032HCID 178457032, 화합물수율 94.1%

시약·촉매·용매 1

HCID 962Water용매

실험 절차

5 ml of ethanol, 5 ml of water and 226 mg of potassium hydroxide were added to 206 mg of N-[1-(2-phenylethyl)-4-ethoxycarbonyl-5-bromopyrazol-3-yl ]-N-[(2'-(1H-tetrazol-5-yl)-biphenyl-4-yl)methyl]-n-propylamine, and heated under reflux for 5 hours. Ethanol was distilled off under reduced pressure, and 10 ml of water were added to the reaction mixture, which was then made acidic with concentrated hydrochloric acid. The resultant was extracted with 50 ml of dichloromethane. After dried over magnesium sulfate, the extract was concentrated under reduced pressure and dried to obtain 185 mg of the intended compound as a pale yellow, amorphous solid.

후처리

  1. temperatureheated
  2. temperatureunder reflux for 5 hours
  3. distillationEthanol was distilled off under reduced pressure, and 10 ml of water
  4. additionwere added to the reaction mixture, which
  5. extractionThe resultant was extracted with 50 ml of dichloromethane
  6. dry with materialAfter dried over magnesium sulfate
  7. concentrationthe extract was concentrated under reduced pressure
  8. customdried

출처 및 근거

ORD 기록
ord-61bfc208f89a443a8da5d1f372ad0aea
출처 데이터셋
uspto-grants-1998_12
특허 번호
US05846991

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