Sodium Carbonate → HCID 54131238, compound

HRID 223208Notes

Reaction equation

HRID 223208 reaction equation
[CH3:1][N:2]1[C:8](=[O:9])[C:7]2[CH:10]=[CH:11][CH:12]=[CH:13][C:6]=2[N:5]2[CH:14]=[N:15][C:16]([C:17]([NH:19][NH2:20])=[O:18])=[C:4]2[CH2:3]1.[N:21]([O-])=O.[Na+].C(=O)([O-])[O-].[Na+].[Na+]>O.C(O)(=O)C>[CH3:1][N:2]1[C:8](=[O:9])[C:7]2[CH:10]=[CH:11][CH:12]=[CH:13][C:6]=2[N:5]2[CH:14]=[N:15][C:16]([C:17]([N:19]=[N+:20]=[N-:21])=[O:18])=[C:4]2[CH2:3]1

Participants

6

Reactant 3

HCID 10340Sodium CarbonateHCID 23668193Sodium NitriteHCID 67713563HCID 67713563, compound

Product 1

HCID 54131238HCID 54131238, compound

Reagents, catalysts & solvents 2

HCID 176Acetic AcidSolventHCID 962WaterSolvent3×

Procedure

A solution of 19 g (70 mmol) of 5,6-dihydro-5-methyl-6-oxo-4H-imidazo[1,5-a][1,4]benzodiazepine-3-carboxylic acid hydrazide in 60 ml of water and 150 ml of glacial acetic acid is treated dropwise at 0° to 5° with a solution of 16.5 g of sodium nitrite in 30 ml of water. The white suspension is subsequently stirred in an ice-bath for 1 hour and cautiously poured into 150 g of sodium carbonate in 400 ml of water. The precipitated material is filtered off under suction, washed with water and dried. There is obtained 5,6-dihydro-5-methyl-6-oxo-4H-imidazo[1,5-a][1,4]benzodiazepine-3-carboxylic acid azide which decomposes at 160°.

Workup

  1. filtrationThe precipitated material is filtered off under suction
  2. washwashed with water
  3. customdried

Sources & evidence

ORD record
ord-1407636d754e420481574485267fd3f6
Source dataset
uspto-grants-1982_10
Patent number
US04352818

Reaction notes

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