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3-Phenyl-2,2-bis(3-(trifluoromethoxy)phenyl)propanenitrile → 3-Phenyl-2,2-bis(3-(trifluoromethoxy)phenyl)propan-1-amine

HRID 511937
Notes
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Reaction equation

HRID 511937 reaction equation
[C:1]1([CH2:7][C:8]([C:22]2[CH:27]=[CH:26][CH:25]=[C:24]([O:28][C:29]([F:32])([F:31])[F:30])[CH:23]=2)([C:11]2[CH:16]=[CH:15][CH:14]=[C:13]([O:17][C:18]([F:21])([F:20])[F:19])[CH:12]=2)[C:9]#[N:10])[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1>CCO.[Ni]>[C:1]1([CH2:7][C:8]([C:11]2[CH:16]=[CH:15][CH:14]=[C:13]([O:17][C:18]([F:19])([F:20])[F:21])[CH:12]=2)([C:22]2[CH:27]=[CH:26][CH:25]=[C:24]([O:28][C:29]([F:32])([F:31])[F:30])[CH:23]=2)[CH2:9][NH2:10])[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1
ParticipantsProcedureWorkupSources & evidenceReaction notes

Participants

4

Reactant 1

HCID 591928133-Phenyl-2,2-bis(3-(trifluoromethoxy)phenyl)propanenitrile

Product 1

HCID 591926393-Phenyl-2,2-bis(3-(trifluoromethoxy)phenyl)propan-1-amineYield 92%

Reagents, catalysts & solvents 2

HCID 935NickelCatalystHCID 702EthanolSolvent

Procedure

To a solution of 3-phenyl-2,2-bis(3-(trifluoromethoxy)phenyl)-propanenitrile (2.20 g, 4.88 mmol), prepared as described in Procedure 15, in EtOH (45 mL) was added an aqueous slurry of Raney 2800 nickel (4 mL). The reaction mixture was stirred under an atmosphere of hydrogen (70 psi) for 42 h. The reaction mixture was filtered through celite and concentrated under reduced pressure to give 3-phenyl-2,2-bis(3-(trifluoromethoxy)phenyl)propan-1-amine (2.04 g, 92% yield) as a clear, colorless oil. LCMS: RT=1.87 min [M+H] 456.2 (2 min Phenomenex Luna C18 column, 4.6×30 mm eluting with 10-90% MeOH/H2O over 2 minutes containing 0.1% TFA; 5 mL/min, monitoring at 220 nm); NMR: 400 MHz 1H (CDCl3) ppm 3.21 (s, 2 H), 3.45 (s, 2 H), 6.59 (d, J=7.03 Hz, 2 H), 6.92 (s, 2 H), 7.01-7.15 (m, 7 H), 7.31 (t, J=8.13 Hz, 2 H).

Workup

  1. filtrationThe reaction mixture was filtered through celite and
  2. concentrationconcentrated under reduced pressure

Sources & evidence

ORD record
ord-022262ed646f426c9513e1f4dabe2af7
Source dataset
uspto-grants-2015_08
DOI
10.6084/m9.figshare.5104873.v1
Patent number
US09102599B2

Reaction notes

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On this pageParticipantsProcedureWorkupSources & evidenceReaction notes