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

HRID 535835Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 535835
[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

Komponenten

4

Edukt 1

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

Produkt 1

HCID 46838908AP-24592Ausbeute 100 %

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 935NickelKatalysatorHCID 887MethanolLösungsmittel

Versuchsvorschrift

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).

Aufarbeitung

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

Quellen und Nachweise

ORD-Eintrag
ord-e1fefc6736ea4d7982d4fc2603595322
Quelldatensatz
uspto-grants-2014_10
Patentnummer
US08859553B2

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