Ammonia → HCID 54277046, compound

HRID 867529Notes

Reaction equation

HRID 867529 reaction equation
[F:1][C:2]1[CH:3]=[CH:4][C:5]2[N:11]3[CH:12]=[N:13][C:14]([C:15]([N:17]4C=CN=C4)=[O:16])=[C:10]3[C@@H:9]3[CH2:22][CH2:23][CH2:24][N:8]3[C:7](=[O:25])[C:6]=2[CH:26]=1.N>CN(C)C=O.O>[F:1][C:2]1[CH:3]=[CH:4][C:5]2[N:11]3[CH:12]=[N:13][C:14]([C:15]([NH2:17])=[O:16])=[C:10]3[C@@H:9]3[CH2:22][CH2:23][CH2:24][N:8]3[C:7](=[O:25])[C:6]=2[CH:26]=1

Participants

5

Reactant 2

HCID 222AmmoniaHCID 53853295HCID 53853295, compound

Product 1

HCID 54277046HCID 54277046, compound

Reagents, catalysts & solvents 2

HCID 962WaterSolvent2×HCID 6228DimethylformamideSolvent

Procedure

20 g (57 mmol) of 1-[[(S)-7-fluoro-11,12,13,13a-tetrahydro-9-oxo-9H-imidazo[1,5-a]pyrrolo[2,1-c][1,4]benzodiazepin-1-yl]carbonyl]imidazole are suspended in 55 ml of N,N-dimethylformamide, the suspension is treated with 9.9 ml of 25 percent ammonia solution in water, the mixture is stirred for a half hour and then poured into 300 ml of water. The precipitated product is filtered off under suction, washed with water and dried at 80° for 48 hours in a water-jet vacuum. There is obtained (S)-7-fluoro-11,12,13,13a-tetrahydro-9-oxo-9H-imidazo[1,5-a]pyrrolo[2,1-c][1,4]benzodiazepine-1-carboxamide of melting point 239°-240°.

Workup

  1. filtrationThe precipitated product is filtered off under suction
  2. washwashed with water
  3. dry with materialdried at 80° for 48 hours in a water-jet vacuum

Sources & evidence

ORD record
ord-e2660cd75582483da7aa2e04f846f88c
Source dataset
uspto-grants-1988_10
Patent number
US04775671

Reaction notes

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