1-Methyl-4-(4-nitro-2-(trifluoromethyl)benzyl)piperazine → AP-24592

HRID 535835ノート

反応式

HRID 535835 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][C:10]=2[C:18]([F:21])([F:20])[F:19])[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][C:10]=2[C:18]([F:21])([F:19])[F:20])[CH2:4][CH2:3]1

参加物

4

反応物 1

HCID 468389061-Methyl-4-(4-nitro-2-(trifluoromethyl)benzyl)piperazine

生成物 1

HCID 46838908AP-24592収率 100%

試薬・触媒・溶媒 2

HCID 935Nickel触媒HCID 887Methanol溶媒

実験手順

Into a solution 4-methyl-1-(4-nitro-2-(trifluoromethyl)benzyl)piperazine (1.5 g, 5 mmol) in MeOH (250 mL) was added Raney Nickel (0.15 g, 10 wt %). The suspension was stirred under hydrogen atmosphere (50 psi) for 24 hrs and monitored by TLC. The reaction mixture was filtered through celite and the filtrate was concentrated under reduced pressure to yield the desired product (1.36 g, 100%). 1H NMR (300 MHz, CDCl3) δ: 7.43-7.46 (1H, d, J=9.0 Hz), 6.91 (1H, s), 6.77-6.80 (1H, d J=9.0 Hz), 3.77 (2H, s), 3.54 (2H, s), 2.53 (8H, brs), 2.34 (3H, s).

後処理

  1. filtrationThe reaction mixture was filtered through celite
  2. concentrationthe filtrate was concentrated under reduced pressure

出典と根拠

ORDレコード
ord-e1fefc6736ea4d7982d4fc2603595322
出典データセット
uspto-grants-2014_10
特許番号
US08859553B2

反応ノート

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