HuagongsheHuagongshe Chemistry Print Report · For research reference only
Sulfur → 4,9-Dihydro-4-methyl-10H-thieno[3,4-b][1,5]benzodiazepin-10-one
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Sulfur | HCID 5362487 | — |
| Reactant | 1,3,4,9-tetrahydro-4-methyl-10H-thieno[3,4-b] [1,5]benzodiazepin-10-one | HCID 12521632 | — |
| Solvent | Chloroform | HCID 6212 | — |
| Product | 4,9-Dihydro-4-methyl-10H-thieno[3,4-b][1,5]benzodiazepin-10-one | HCID 12521642 | — |
Reaction Steps
A mixture of 0.5 g. of 1,3,4,9-tetrahydro-4-methyl-10H-thieno[3,4-b][1,5]benzodiazepin-10-one and 0.5 g. of sulfur is fused at 160° C. ± 5 for 1 hour. The fusion mixture is slurried with chloroform and filtered. The filtrate is chromatographed on silica gel with benzene:methanol 9:1 to give a solid, which is recrystallized from methanol-water to give a tan solid, m.p. 224°-225° C. (dec.).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US04007272 |
| Source dataset | uspto-grants-1977_02 |
| ORD ID | ord-6fa6c95a255e476f96f40dca3d58a551 |
| Source note | uspto-grants-1977_02 |