p-Fluoronitrobenzene → 1-Methyl-4-(4-nitrophenyl)piperazine

HRID 238501ノート

反応式

HRID 238501 の反応式
F[C:2]1[CH:7]=[CH:6][C:5]([N+:8]([O-:10])=[O:9])=[CH:4][CH:3]=1.[CH3:11][N:12]1[CH2:17][CH2:16][NH:15][CH2:14][CH2:13]1>>[CH3:11][N:12]1[CH2:17][CH2:16][N:15]([C:2]2[CH:7]=[CH:6][C:5]([N+:8]([O-:10])=[O:9])=[CH:4][CH:3]=2)[CH2:14][CH2:13]1

参加物

3

反応物 2

HCID 9590p-FluoronitrobenzeneHCID 531671-Methylpiperazine

生成物 1

HCID 28251981-Methyl-4-(4-nitrophenyl)piperazine収率 77.3%

反応条件

温度
90 °C

実験手順

1-Fluoro-4-nitrobenzene (3.0 g, 0.021 mol) and 1-methylpiperazine (6.98 ml, 0.63 mol) were combined and heated neat at 90° C. for 48 h. Upon cooling to RT, the resulting brown oil solidified. The crude material was purified by re-crystallization from EtOAc/Hexane mixtures to leave the title compound as an orange solid (3.59 g). MS: (ES+) 222 (M+1)+; (ES−): 220 (M−1)−. Calc'd for C11H15N3O2: 221.12.

後処理

  1. temperatureUpon cooling to RT
  2. customThe crude material was purified by re-crystallization from EtOAc/Hexane mixtures

出典と根拠

ORDレコード
ord-42a65be9598d4c9ea6bf08abce16b63f
出典データセット
uspto-grants-2014_02
特許番号
US08642624B2

反応ノート

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