Hydrochloric Acid → HCID 22819141, compound

HRID 867525Notes

Reaction equation

HRID 867525 reaction equation
[Cl:1][C:2]1[C:7]2[C:8](=[O:26])[N:9]3[CH2:25][CH2:24][CH2:23][C@H:10]3[C:11]3[N:12]([CH:13]=[N:14][C:15]=3[C:16]([O:18]C(C)(C)C)=[O:17])[C:6]=2[CH:5]=[CH:4][C:3]=1[F:27].Cl>>[Cl:1][C:2]1[C:7]2[C:8](=[O:26])[N:9]3[CH2:25][CH2:24][CH2:23][C@H:10]3[C:11]3[N:12]([CH:13]=[N:14][C:15]=3[C:16]([OH:18])=[O:17])[C:6]=2[CH:5]=[CH:4][C:3]=1[F:27]

Participants

3

Reactant 2

HCID 313Hydrochloric AcidHCID 70040464HCID 70040464, compound

Product 1

HCID 22819141HCID 22819141, compound

Procedure

A mixture of 4.7 g (12 mmol) of t-butyl (S)-8-chloro-7-fluoro-11,12,13,13a-tetrahydro-9-oxo-9H-imidazo[1,5-a]pyrrolo[2,1-c][1,4]benzodiazepine-1-carboxylate and 24 ml of 1N hydrochloric acid is heated to boiling under reflux for 1.5 hours. The mixture is then cooled to about 5°, the product is filtered off under suction, rinsed with water and dried at 85° in vacuo. There is obtained (S)-8-chloro-7-fluoro-11,12,13,13a-tetrahydro-9-oxo-9H-imidazo[1,5-a]pyrrolo[2,1-c][1,4]benzodiazepine-1-carboxylic acid of decomposition point 261°-263°.

Workup

  1. temperatureis heated
  2. temperatureunder reflux for 1.5 hours
  3. temperatureThe mixture is then cooled to about 5°
  4. filtrationthe product is filtered off under suction
  5. washrinsed with water
  6. customdried at 85° in vacuo

Sources & evidence

ORD record
ord-de4e922149d845b8a15c7e7d1682d9ec
Source dataset
uspto-grants-1988_10
Patent number
US04775671

Reaction notes

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