Water → 4-(4-Indan-2-yl-piperazin-1-yl)benzoic acid ethyl ester

HRID 1977299

反応式

HRID 1977299 の反応式
Cl.Cl.[CH2:3]([O:5][C:6](=[O:19])[C:7]1[CH:12]=[CH:11][C:10]([N:13]2[CH2:18][CH2:17][NH:16][CH2:15][CH2:14]2)=[CH:9][CH:8]=1)[CH3:4].C(=O)(O)[O-].[K+].[CH2:25]1[C:33]2[C:28](=[CH:29][CH:30]=[CH:31][CH:32]=2)[CH2:27][CH:26]1OS(C)(=O)=O.O>C(#N)C>[CH2:3]([O:5][C:6](=[O:19])[C:7]1[CH:8]=[CH:9][C:10]([N:13]2[CH2:14][CH2:15][N:16]([CH:26]3[CH2:25][C:33]4[C:28](=[CH:29][CH:30]=[CH:31][CH:32]=4)[CH2:27]3)[CH2:17][CH2:18]2)=[CH:11][CH:12]=1)[CH3:4]

参加物

6

反応物 4

HCID 962WaterHCID 2552212,3-Dihydro-1h-inden-2-yl methanesulfonateHCID 516893Potassium BicarbonateHCID 700526324-Piperazin-1-yl-benzoic acid ethyl ester dihydrochloride

生成物 1

HCID 700560464-(4-Indan-2-yl-piperazin-1-yl)benzoic acid ethyl ester収率 33.4%

試薬・触媒・溶媒 1

HCID 6342Acetonitrile溶媒

実験手順

To a suspension of 4-piperazin-1-yl-benzoic acid ethyl ester dihydrochloride (1 g) and potassium bicarbonate (1.57 g) in acetonitrile (10 ml) was added methanesulfonic acid indane-2-yl ester (0.69 g) and the mixture was stirred under refluxing for 8 hours. The reaction mixture was pulverized with water. The precipitate was collected by filtration and dried over under reduced pressure. The powder was purified by column chromatography on silica gel using methanol/dichloromethane (50:1) as the eluent to give 4-(4-indan-2-yl-piperazin-1-yl)benzoic acid ethyl ester (0.38 g).

後処理

  1. temperatureunder refluxing for 8 hours
  2. filtrationThe precipitate was collected by filtration
  3. customdried over under reduced pressure
  4. customThe powder was purified by column chromatography on silica gel

出典と根拠

ORDレコード
ord-c7c5d80d58da4ba2bdaa017df586efd2
出典データセット
uspto-grants-2001_05
特許番号
US06232290B1

関連ノート

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