Hydrochloric Acid → HCID 54415726, compound

HRID 223223Notes

Reaction equation

HRID 223223 reaction equation
[O:1]=[C:2]1[C:8]2[CH:9]=[CH:10][CH:11]=[CH:12][C:7]=2[N:6]2[CH:13]=[N:14][C:15]([C:16]([O:18]CC)=[O:17])=[C:5]2[C@@H:4]2[CH2:21][CH2:22][CH2:23][N:3]12.[OH-].[Na+].Cl>C(O)C.O>[O:1]=[C:2]1[C:8]2[CH:9]=[CH:10][CH:11]=[CH:12][C:7]=2[N:6]2[CH:13]=[N:14][C:15]([C:16]([OH:18])=[O:17])=[C:5]2[C@@H:4]2[CH2:21][CH2:22][CH2:23][N:3]12

Participants

6

Reactant 3

HCID 313Hydrochloric AcidHCID 14798Sodium HydroxideHCID 10041121Ethyl (7S)-12-oxo-2,4,11-triazatetracyclo[11.4.0.02,6.07,11]heptadeca-1(17),3,5,13,15-pentaene-5-carboxylate

Product 1

HCID 54415726HCID 54415726, compound

Reagents, catalysts & solvents 2

HCID 702EthanolSolventHCID 962WaterSolvent

Procedure

A solution of 12.45 g (0.04 mol) of ethyl (S)-11,12,13,13a-tetrahydro-9-oxo-9H-imidazo[1,5-a]pyrrolo[2,1-c][1,4]benzodiazepine-1-carboxylate and 1.6 g (0.04 mol) of sodium hydroxide in 100 ml of ethanol and 25 ml of water is heated to boiling under reflux for 30 minutes. Subsequently, 40 ml of 1 N hydrochloric acid are added thereto and the mixture is evaporated to half of the volume. The crystals which thereby precipitate are filtered off under suction, washed with water and dried. There is obtained (S)-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 225°.

Workup

  1. temperatureunder reflux for 30 minutes
  2. customthe mixture is evaporated to half of the volume
  3. filtrationThe crystals which thereby precipitate are filtered off under suction
  4. washwashed with water
  5. customdried

Sources & evidence

ORD record
ord-a35ceba80900478aa0b48ecfc18b522c
Source dataset
uspto-grants-1982_10
Patent number
US04352818

Reaction notes

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