Water → HCID 70394522, compound

HRID 1606978Notes

Reaction equation

HRID 1606978 reaction equation
[Br:1][C:2]1[C:7]2[C:8](=O)[N:9]3[CH2:21][CH2:20][CH2:19][C@H:10]3[C:11]3[N:12]([CH:13]=[N:14][C:15]=3C(O)=O)[C:6]=2[CH:5]=[CH:4][CH:3]=1.[OH2:23]>CN(C)C=O>[Br:1][C:2]1[C:7]2[CH2:8][N:9]3[CH2:21][CH2:20][CH2:19][C@H:10]3[CH:11]3[C:15](=[O:23])[N:14]=[CH:13][N:12]3[C:6]=2[CH:5]=[CH:4][CH:3]=1

Participants

4

Reactant 2

HCID 962WaterHCID 22821777HCID 22821777, compound

Product 1

HCID 70394522HCID 70394522, compound

Reagents, catalysts & solvents 1

HCID 6228DimethylformamideSolvent

Procedure

109.03 g (300 mmol) of (S)-8-bromo-11,12,13,13a-tetrahydro-9-oxo-9H-imidazo[1,5-a]pyrrolo[2,1-c][1,4]benzodiazepine-1-carboxylic acid was decarboxylated at 290°. The melt was dissolved in about 400 ml of N,N-dimethylformamide and the solution was poured into 2.5 l of water. After stirring for 30 minutes the precipitated product was filtered off, rinsed with water and dried. There was obtained (S)-8-bromo-11,12,13,13a-tetrahydro-9H-imidazo[1,5-a]pyrrolo[2,1-c][1,4]benzodiazepine-one of melting point 232°-233°.

Workup

  1. customwas decarboxylated at 290°
  2. filtrationwas filtered off
  3. washrinsed with water
  4. customdried

Sources & evidence

ORD record
ord-678d2f3e61b64a0ab31391a7c6f422a2
Source dataset
uspto-grants-1989_09
Patent number
US04863920

Reaction notes

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