Piperazine → 3-Methylbenzylpiperazine

HRID 893286ノート

反応式

HRID 893286 の反応式
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

参加物

5

反応物 2

HCID 4837PiperazineHCID 12099m-Xylyl bromide

生成物 1

HCID 792133-Methylbenzylpiperazine収率 78.1%

試薬・触媒・溶媒 2

HCID 241Benzene溶媒HCID 3283Diethyl Ether溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-c6e0b8d02e2348fcb55532b1fe88386d
出典データセット
uspto-grants-1992_06
特許番号
US05124330

反応ノート

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