Water → HCID 53853295, compound

HRID 867528Notes

Reaction equation

HRID 867528 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](O)=[O:16])=[C:10]3[C@@H:9]3[CH2:18][CH2:19][CH2:20][N:8]3[C:7](=[O:21])[C:6]=2[CH:22]=1.O>CN(C)C=O>[F:1][C:2]1[CH:3]=[CH:4][C:5]2[N:11]3[CH:12]=[N:13][C:14]([C:15]([N:11]4[CH:10]=[CH:14][N:13]=[CH:12]4)=[O:16])=[C:10]3[C@@H:9]3[CH2:18][CH2:19][CH2:20][N:8]3[C:7](=[O:21])[C:6]=2[CH:22]=1

Participants

4

Reactant 2

HCID 962WaterHCID 54510081HCID 54510081, compound

Product 1

HCID 53853295HCID 53853295, compound

Reagents, catalysts & solvents 1

HCID 6228DimethylformamideSolvent

Procedure

14.53 g (89.6 mmol) of N,N'-carbonyldiimidazole are introduced portion wise into a suspension of 20 g (66.4 mmol) of (S)-7-fluoro-11,12,13,13a-tetrahydro-9-oxo-9H-imidazo[1,5-a]pyrrolo[2,1-c][1,4]benzodiazepine-1-carboxylic acid in 70 ml of N,N-dimethylformamide. The solution obtained is stirred at room temperature and at 50°, in each case for 1 hour, and is then poured into about 300 ml of water. After stirring for 20 minutes the suspension obtained is suction filtered and the residue is washed with water. After drying at 90° for 16 hours in a water-jet vacuum there is obtained 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 of melting point 206°-207°.

Workup

  1. customThe solution obtained
  2. stirringAfter stirring for 20 minutes the suspension
  3. customobtained
  4. filtrationfiltered
  5. washthe residue is washed with water
  6. dry with materialAfter drying at 90° for 16 hours in a water-jet vacuum

Sources & evidence

ORD record
ord-fd88989dc7464878ae81a558552294d5
Source dataset
uspto-grants-1988_10
Patent number
US04775671

Reaction notes

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