Methanol → HCID 19763361, compound

HRID 373798Notes

Reaction equation

HRID 373798 reaction equation
CO.[N:3](=[C:5]1[C:11]2[CH:12]=[N:13][CH:14]=[N:15][C:10]=2[C:9]2[CH:16]=[CH:17][CH:18]=[CH:19][C:8]=2[C:7]([C:20]2[CH:25]=[CH:24][CH:23]=[CH:22][CH:21]=2)=[N:6]1)O>C(O)C.[Ni]>[NH2:3][CH:5]1[C:11]2[CH:12]=[N:13][CH:14]=[N:15][C:10]=2[C:9]2[CH:16]=[CH:17][CH:18]=[CH:19][C:8]=2[C:7]([C:20]2[CH:21]=[CH:22][CH:23]=[CH:24][CH:25]=2)=[N:6]1

Participants

5

Reactant 2

HCID 887MethanolHCID 1360725937-Phenyl-5H-pyrimido[5,4-d][2]benzazepin-5-one oxime

Product 1

HCID 19763361HCID 19763361, compound

Reagents, catalysts & solvents 2

HCID 935NickelCatalystHCID 702EthanolSolvent

Procedure

A solution of 150 ml of methanol containing 5 g of 5-oximino-7-phenyl-5H-pyrimido[5,4-d][2]-benzazepine is treated with a slurry of active Raney-Nickel catalyst1 in ethanol (10 g). The resulting suspension is hydrogenated on a Parr apparatus at 60 psi and 23° C. for about 30 hours. The catalyst is removed by filtration and the filtrate is concentrated to afford the title compound.

Workup

  1. customThe catalyst is removed by filtration
  2. concentrationthe filtrate is concentrated

Sources & evidence

ORD record
ord-2a49148b0a5c4c748b515e0378765ed3
Source dataset
uspto-grants-1992_11
Patent number
US05166151

Reaction notes

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