Hydrochloric Acid → Ro 15-3890

HRID 223203Notes

Reaction equation

HRID 223203 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:17]CC)=[O:16])=[C:10]3[CH2:9][N:8]([CH3:20])[C:7](=[O:21])[C:6]=2[CH:22]=1.[OH-].[Na+].Cl>C(O)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]([OH:17])=[O:16])=[C:10]3[CH2:9][N:8]([CH3:20])[C:7](=[O:21])[C:6]=2[CH:22]=1

Participants

6

Reactant 3

HCID 313Hydrochloric AcidHCID 3373FlumazenilHCID 14798Sodium Hydroxide

Product 1

HCID 134757Ro 15-3890

Reagents, catalysts & solvents 2

HCID 702EthanolSolventHCID 962WaterSolvent

Procedure

A solution of 3.03 g (10 mmol) of ethyl 8-fluoro-5,6-dihydro-5-methyl-6-oxo-4H-imidazo[1,5-a][1,4]-benzodiazepine-3-carboxylate and 0.44 g (11 mmol) of sodium hydroxide in 20 ml of ethanol and 10 ml of water is heated to boiling under reflux for 30 minutes. Subsequently, the mixture is treated with 11 ml of 1 N hydrochloric acid and concentrated to half of the volume. The precipitated crystals are filtered off under suction and dried. There is obtained 8-fluoro-5,6-dihydro-5-methyl-6-oxo-4H-imidazo[1,5-a][1,4]benzodiazepine-3-carboxylic acid of decomposition point 279°.

Workup

  1. temperatureunder reflux for 30 minutes
  2. concentrationconcentrated to half of the volume
  3. filtrationThe precipitated crystals are filtered off under suction
  4. customdried

Sources & evidence

ORD record
ord-4eefd3d7ea264acea23a529a6a2cc491
Source dataset
uspto-grants-1982_10
Patent number
US04352818

Reaction notes

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