Triethylamine → Cyclopentanecarbonyl 4-(methyl)phenyl piperazine

HRID 417995노트

반응식

HRID 417995 반응식
Cl.Cl.[CH3:3][C:4]1[CH:9]=[CH:8][C:7]([N:10]2[CH2:15][CH2:14][NH:13][CH2:12][CH2:11]2)=[CH:6][CH:5]=1.CCN(CC)CC.[CH:23]1([C:28](Cl)=[O:29])[CH2:27][CH2:26][CH2:25][CH2:24]1>C(Cl)Cl>[CH:23]1([C:28]([CH:11]2[CH2:12][NH:13][CH2:14][CH2:15][N:10]2[C:7]2[CH:6]=[CH:5][C:4]([CH3:3])=[CH:9][CH:8]=2)=[O:29])[CH2:27][CH2:26][CH2:25][CH2:24]1

참가 물질

5

반응물 3

HCID 8471TriethylamineHCID 78284Cyclopentanecarbonyl chlorideHCID 831121-(p-Tolyl)piperazine dihydrochloride

생성물 1

HCID 66650881Cyclopentanecarbonyl 4-(methyl)phenyl piperazine수율 98.3%

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

4-Methylphenyl piperazine dihydrochloride (4.20 g, 16.9 mmol) and NEt3 (7.0 mL, 50.2 mmol) were dissolved in DCM (125 mL) at 0° C. Cyclopentanecarbonyl chloride (2.0 mL, 16.5 mmol) was added and the reaction mixture was allowed to warm to room temperature over 16 hours. The reaction mixture was washed with 1M aq Na2CO3 solution (3×100 mL), dried (MgSO4) and concentrated in vacuo to give cyclopentanecarbonyl 4-(methyl)phenyl piperazine (4.42 g, 98%) as a pale brown oil which was used without further purification.

후처리

  1. washThe reaction mixture was washed with 1M aq Na2CO3 solution (3×100 mL)
  2. dry with materialdried (MgSO4)
  3. concentrationconcentrated in vacuo

출처 및 근거

ORD 기록
ord-3297df9f01b645ad96f977418a0a8f14
출처 데이터셋
uspto-grants-2012_01
특허 번호
US08093248B2

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