1-Methyl-4-(4-nitrobenzyl)piperazine → 4-((4-Methylpiperazin-1-yl)methyl)aniline

HRID 501220

反応式

HRID 501220 の反応式
[CH3:1][N:2]1[CH2:7][CH2:6][N:5]([CH2:8][C:9]2[CH:14]=[CH:13][C:12]([N+:15]([O-])=O)=[CH:11][CH:10]=2)[CH2:4][CH2:3]1>CO.[Ni]>[CH3:1][N:2]1[CH2:7][CH2:6][N:5]([CH2:8][C:9]2[CH:14]=[CH:13][C:12]([NH2:15])=[CH:11][CH:10]=2)[CH2:4][CH2:3]1

参加物

4

反応物 1

HCID 6777951-Methyl-4-(4-nitrobenzyl)piperazine

生成物 1

HCID 31539964-((4-Methylpiperazin-1-yl)methyl)aniline収率 91.7%

試薬・触媒・溶媒 2

HCID 935Nickel触媒HCID 887Methanol溶媒

実験手順

To a solution of 1-methyl-4-(4-nitrobenzyl)piperazine (4.0 g) in methanol (100 mL) at room temperature under nitrogen atmosphere was added Raney nickel (1.6 gm). The reaction mixture was stirred for 2 hr under hydrogen atmosphere. The progress of the reaction was monitored by TLC and upon completion of the reaction, the mixture was filtered under nitrogen atmosphere and the solvent was removed under reduced pressure to give 4-[(4-methylpiperazin-1-yl)methyl]aniline (3.2 g). 1H NMR (CDCl3, 200 MHz) δ: 7.13 (2H, d, J=8.4 Hz), 6.61 (2H, d, J=8.4 Hz), 3.41 (2H, s), 2.45 (8H, bm), 2.27 (3H, s); m/e=206 (M+1).

後処理

  1. customThe progress of the reaction was monitored by TLC and upon completion of the reaction
  2. filtrationthe mixture was filtered under nitrogen atmosphere
  3. customthe solvent was removed under reduced pressure

出典と根拠

ORDレコード
ord-ac0874e7ff6c46658b2fe821ad1c95e2
出典データセット
uspto-grants-2010_08
特許番号
US07772245B2

関連ノート

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