Water → 1-Benzyl-4-(4-nitrophenyl)piperazine

HRID 479378

반응식

HRID 479378 반응식
[CH2:1]([N:8]1[CH2:13][CH2:12][NH:11][CH2:10][CH2:9]1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.C(=O)([O-])[O-].[K+].[K+].Cl[C:21]1[CH:26]=[CH:25][C:24]([N+:27]([O-:29])=[O:28])=[CH:23][CH:22]=1.O>CN(C)C=O>[CH2:1]([N:8]1[CH2:13][CH2:12][N:11]([C:21]2[CH:26]=[CH:25][C:24]([N+:27]([O-:29])=[O:28])=[CH:23][CH:22]=2)[CH2:10][CH2:9]1)[C:2]1[CH:3]=[CH:4][CH:5]=[CH:6][CH:7]=1

참가 물질

6

반응물 4

HCID 962WaterHCID 74741-Chloro-4-nitrobenzeneHCID 11430Potassium CarbonateHCID 759941-Benzylpiperazine

생성물 1

HCID 27474271-Benzyl-4-(4-nitrophenyl)piperazine수율 76%

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

1-Benzylpiperazine (2.8 ml; 16 mmol) and potassium carbonate (2.3 g; 17 mmol) were added to a solution of 1-chloro-4-nitrobenzene (2.0 g; 13 mmol) in dimethylformamide (0.5 ml), and the mixture was stirred for 7 hours in a bath controlled at 100° C. Water was added to the reaction mixture to conduct extraction with chloroform. The organic layer was washed with saturated brine, dried over anhydrous sodium sulfate and then concentrated under reduced pressure. The resultant crude oil was purified by column chromatography on silica gel, thereby obtaining 2.9 g (yield: 76%) of 4-(4-benzyl-1-piperazinyl)-1-nitrobenzene as a colorless oil.

후처리

  1. customcontrolled at 100° C
  2. extractionextraction with chloroform
  3. washThe organic layer was washed with saturated brine
  4. dry with materialdried over anhydrous sodium sulfate
  5. concentrationconcentrated under reduced pressure
  6. customThe resultant crude oil was purified by column chromatography on silica gel

출처 및 근거

ORD 기록
ord-a06b0b315d3441e6a2b53be2ed8f3193
출처 데이터셋
uspto-grants-2003_11
특허 번호
US06645957B2

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