Ethanol → HCID 178457032、化合物

HRID 399354ノート

反応式

HRID 399354 の反応式
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

参加物

5

反応物 3

HCID 702EthanolHCID 14797Potassium HydroxideHCID 178457033HCID 178457033、化合物

生成物 1

HCID 178457032HCID 178457032、化合物収率 94.1%

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-29d410be47cc4f30a7c8d8ab6051de54
出典データセット
uspto-grants-1998_10
特許番号
US05817828

反応ノート

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