Piperazine → 3-Methylbenzylpiperazine

HRID 893286노트

반응식

HRID 893286 반응식
Br[CH2:2][C:3]1[CH:8]=[CH:7][CH:6]=[C:5]([CH3:9])[CH:4]=1.[NH:10]1[CH2:15][CH2:14][NH:13][CH2:12][CH2:11]1>C1C=CC=CC=1.C(OCC)C>[CH3:9][C:5]1[CH:4]=[C:3]([CH:8]=[CH:7][CH:6]=1)[CH2:2][N:10]1[CH2:15][CH2:14][NH:13][CH2:12][CH2:11]1

참가 물질

5

반응물 2

HCID 4837PiperazineHCID 12099m-Xylyl bromide

생성물 1

HCID 792133-Methylbenzylpiperazine수율 78.1%

시약·촉매·용매 2

HCID 241Benzene용매HCID 3283Diethyl Ether용매

실험 절차

α-Bromo-m-xylene (10 ml, 74 mmole) was added to a solution of 75 g (11.8 equiv.) of anhydrous piperazine in 500 ml of benzene and the reaction was heated to reflux for two hours. After cooling to room temperature, the reaction was diluted with 300 ml of diethyl ether and washed with 500 ml of 0.2 M sodium hydroxide followed by two 500 ml portions of water. The organic solution was dried over sodium sulfate and the solvent removed to give 11.0 g (78%) of crude 1-(3-methylbenzyl)piperazine as a colorless oil.

후처리

  1. temperaturethe reaction was heated
  2. temperatureto reflux for two hours
  3. washwashed with 500 ml of 0.2 M sodium hydroxide
  4. dry with materialThe organic solution was dried over sodium sulfate
  5. customthe solvent removed

출처 및 근거

ORD 기록
ord-c6e0b8d02e2348fcb55532b1fe88386d
출처 데이터셋
uspto-grants-1992_06
특허 번호
US05124330

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