HCID 54511962, compound → HCID 21201707, compound

HRID 1979343Notes

Reaction equation

HRID 1979343 reaction equation
[CH3:1][O:2][CH2:3][N:4]1[C:10]2[CH:11]=[CH:12][CH:13]=[CH:14][C:9]=2[N:8]([C:15]2[CH:20]=[CH:19][CH:18]=[CH:17][C:16]=2[F:21])[CH2:7][C:6](=[N:22]OC(NCCC)=O)[C:5]1=[O:30]>CO.[C].[Pd]>[CH3:1][O:2][CH2:3][N:4]1[C:10]2[CH:11]=[CH:12][CH:13]=[CH:14][C:9]=2[N:8]([C:15]2[CH:20]=[CH:19][CH:18]=[CH:17][C:16]=2[F:21])[CH2:7][CH:6]([NH2:22])[C:5]1=[O:30]

Participants

4

Reactant 1

HCID 54511962HCID 54511962, compound

Product 1

HCID 21201707HCID 21201707, compoundYield 25%

Reagents, catalysts & solvents 2

HCID 178418390HCID 178418390, compoundCatalystHCID 887MethanolSolvent

Procedure

1-Methoxymethyl-2-oxo-3-propylaminocarbonyloxyimino-5-(2-fluorophenyl)-1,3,4,5-tetrahydro-2H-1,5-benzodiazepine (2.52 g) was dissolved in methanol (30 ml), 10% palladium carbon (0.60 g) was added thereto, the mixture was swung for 4 hours under hydrogen atmosphere (3.5-3.0 kg/cm2). Palladium carbon was removed by filtration, the filtrate was concentrated under reduced pressure, and the residue was purified by silica gel column chromatography (chloroform:methanol=20:1), to thereby obtain 0.48 g of the titled compound as yellow-brown amorphous.

Workup

  1. customPalladium carbon was removed by filtration
  2. concentrationthe filtrate was concentrated under reduced pressure
  3. customthe residue was purified by silica gel column chromatography (chloroform:methanol=20:1)

Sources & evidence

ORD record
ord-01a7da4a44ef424389db34431164670a
Source dataset
uspto-grants-2001_05
Patent number
US06239131B1

Reaction notes

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