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

HRID 535835노트

반응식

HRID 535835 반응식
[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

참가 물질

4

반응물 1

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

생성물 1

HCID 46838908AP-24592수율 100%

시약·촉매·용매 2

HCID 935Nickel촉매HCID 887Methanol용매

실험 절차

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).

후처리

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

출처 및 근거

ORD 기록
ord-e1fefc6736ea4d7982d4fc2603595322
출처 데이터셋
uspto-grants-2014_10
특허 번호
US08859553B2

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