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

HRID 1977299

반응식

HRID 1977299 반응식
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]

참가 물질

6

반응물 4

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

생성물 1

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

시약·촉매·용매 1

HCID 6342Acetonitrile용매

실험 절차

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).

후처리

  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

출처 및 근거

ORD 기록
ord-c7c5d80d58da4ba2bdaa017df586efd2
출처 데이터셋
uspto-grants-2001_05
특허 번호
US06232290B1

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