HuagongsheHuagongshe Chemistry Print Report · For research reference only
Hydrogen Sulfide → HCID 21842253, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Hydrogen Sulfide | HCID 402 | — |
| Reactant | 8-fluoro-5-methyl-6-oxo-5,6-dihydro-4H-imidazo[1,5-a][1,4]benzodiazepine-3-carbonitrile | HCID 9881542 | — |
| Solvent | Pyridine | HCID 1049 | — |
| Solvent | Triethylamine | HCID 8471 | — |
| Product | HCID 21842253 | HCID 21842253 | 91% |
Reaction Steps
A stream of hydrogen sulphide was conducted for 1/2 hr. through a solution of 4.4 g (0.0172 mol) of 8-fluoro-5-methyl-6-oxo-5,6-dihydro-4H-imidazo[1,5-a][1,4]benzodiazepine-3-carbonitrile in 100 ml of pyridine and 1 ml of triethylamine. The dark green solution was left to stand for 64 hrs., then de-gassed with a stream of nitrogen and subsequently completely freed from the solvents. The residue was partitioned between dichloromethane/tetrahydrofuran and water, extracted, concentrated, stirred vigorously in ether and filtered off under suction. There were obtained 4.55 g (91%) of 8-fluoro-5-methyl-6-oxo-5,6-dihydro-4H-imidazo[1,5-a][1,4]benzodiazepine-3-thiocarboxamide as yellow crystals.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US05885986 |
| Source dataset | uspto-grants-1999_03 |
| ORD ID | ord-5fab9f1022e64e40b1875e3939435aa9 |
| Source note | uspto-grants-1999_03 |