HuagongsheHuagongshe Chemistry Print Report · For research reference only
Methanol → HCID 13282024, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Methanol | HCID 887 | — |
| Reactant | Sodium borohydride | HCID 4311764 | — |
| Reactant | HCID 13282025 | HCID 13282025 | — |
| Reactant | HCID 178418361 | HCID 178418361 | — |
| Product | HCID 13282024 | HCID 13282024 | 35% |
Reaction Steps
4,9-Dihydro-4-isonicotinoyl-10H-thieno[3,4-b][1,5]benzodiazepin-10-one methoiodide in an amount of 3.4 gm (0.0073 mol) was suspended in 40 ml of methanol, and at 0° C. 0.5 gm (0.014 mol) of sodium borohydride were added in portions. After the development of hydrogen ceased, the mixture was stirred for a further two hours in an ice bath. Then, 100 ml of ice-water was added, the mixture was filtered, and the filtrate was extracted with methylene chloride. The extraction residue was recrystallized from acetonitrile. 4,9-Dihydro-4-[(1-methyl-1,2,5,6-tetrahydro-4-pyridinyl)carbonyl]-10H-thieno[3,4-b][1,5]benzodiazepin-10-one was obtained, m.p.: 210°-212° C., in a yield of 35% of theory.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US04424225 |
| Source dataset | uspto-grants-1984_01 |
| ORD ID | ord-65fd053294714d9c9e6f878a353d9a79 |
| Source note | uspto-grants-1984_01 |