Methane → HCID 19830647, compound

HRID 1606975Notes

Reaction equation

HRID 1606975 reaction equation
[Br:1][C:2]1[C:7]2[C:8](=[O:20])[N:9]([CH3:19])[CH2:10][C:11]3[N:12]([CH:13]=[N:14][C:15]=3C(O)=O)[C:6]=2[CH:5]=[CH:4][CH:3]=1.C>C(Cl)Cl.C(OCC)(=O)C.C(O)C>[Br:1][C:2]1[C:7]2[C:8](=[O:20])[N:9]([CH3:19])[CH2:10][C:11]3[N:12]([CH:13]=[N:14][CH:15]=3)[C:6]=2[CH:5]=[CH:4][CH:3]=1

Participants

6

Reactant 2

HCID 297MethaneHCID 22914630HCID 22914630, compound

Product 1

HCID 19830647HCID 19830647, compound

Reagents, catalysts & solvents 3

HCID 702EthanolSolventHCID 6344DichloromethaneSolventHCID 8857Ethyl AcetateSolvent

Procedure

19.1 g (56.8 mmol) of 7-bromo-5,6-dihydro-5-methyl-6-oxo-4H-imidazo[1,5-a][1,4]benzodiazepine-3-carboxylic acid are decarboxylated at 290°-300°. The melt was taken up in methylene chloride, the solution was diluted with ethyl acetate and ethanol and decolorized with animal charcoal. After evaporation and recrystallization from ethyl acetate and ethanol there was obtained 7-bromo-4,5-dihydro-5-methyl-6H-imidazo[1,5-a][1,4]benzodiazepin-6-one of melting point 196°-197°.

Workup

  1. customare decarboxylated at 290°-300°
  2. customAfter evaporation and recrystallization from ethyl acetate

Sources & evidence

ORD record
ord-80c94a6635ff4deab5a0530a0dcd5f86
Source dataset
uspto-grants-1989_09
Patent number
US04863920

Reaction notes

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