Carbon Dioxide → HCID 70394981, compound
Reaction equation
[CH3:1][N:2]1[C:8](=O)[C:7]2[CH:10]=[CH:11][S:12][C:6]=2[N:5]2[CH:13]=[N:14][C:15](C(O)=O)=[C:4]2[CH2:3]1.C(=O)=[O:20]>ClC(Cl)Cl>[CH3:1][N:2]1[CH2:8][C:7]2[CH:10]=[CH:11][S:12](=[O:20])[C:6]=2[N:5]2[CH:13]=[N:14][CH:15]=[C:4]2[CH2:3]1Participants
4
Reactant 2
Product 1
Reagents, catalysts & solvents 1
Procedure
27 g of 5,6-dihydro-5-methyl-4-oxo-4H-imidazo[1,5-a]thieno[3,2-f][1,4]diazepine-7-carboxylic acid was immersed in a flask filled with argon in a heating bath pre-heated to 280°. The substance melts with decarboxylation. After completion of the evolution of carbon dioxide (about 7 to 8 min.) the flask was cooled slightly. Even before it had solidified, the reaction mixture was mixed with 250 ml of trichloromethane. The solution was evaporated in a vacuum and the residue was recrystallized from ethyl acetate/diisopropyl ether. There was obtained 5,6-dihydro-5-methyl-4H-imidazo[1,5-a]thieno[3,2-f][1,4]diazepine-one of melting point 160°-163°. After recrystallization from ethyl acetate the melting point was 163°-164°.
Workup
- additionfilled with argon in a heating bath
- temperaturepre-heated to 280°
- customThe solution was evaporated in a vacuum
- customthe residue was recrystallized from ethyl acetate/diisopropyl ether
Sources & evidence
- ORD record
- ord-8792875ba4a64d0caf9ccc50f932b4a5
- Source dataset
- uspto-grants-1989_09
- Patent number
- US04863920
Reaction notes
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