Methane → HCID 19830647, compound

HRID 1493130Notes

Reaction equation

HRID 1493130 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 were 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. customwere decarboxylated at 290-300°
  2. customAfter evaporation and recrystallization from ethyl acetate

Sources & evidence

ORD record
ord-a57eff01d13b4ca3bf0616abb6a79e91
Source dataset
uspto-grants-1991_06
Patent number
US05021411

Reaction notes

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