Piperazine → 3-Methylbenzylpiperazine

HRID 2379681노트

반응식

HRID 2379681 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 0.2M 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 0.2M sodium hydroxide
  4. dry with materialThe organic solution was dried over sodium sulfate
  5. customthe solvent removed

출처 및 근거

ORD 기록
ord-2acf3d57b6d446d6aa6834b7491257be
출처 데이터셋
uspto-grants-1994_11
특허 번호
US05364843

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