HuagongsheHuagongshe Chemistry Print Report · For research reference only
Sodium Sulfate → 6-Chloro-2,3,4,5-tetrahydro-1,4-benzothiazepine
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Sodium Sulfate | HCID 24436 | — |
| Reactant | 6-Chloro-4,5-dihydro-1,4-benzothiazepin-3(2H)-one | HCID 10220003 | — |
| Reactant | Aluminium lithium hydride | HCID 21226445 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | 6-Chloro-2,3,4,5-tetrahydro-1,4-benzothiazepine | HCID 10198105 | — |
Reaction Steps
6-Chloro-4,5-dihydro-1,4-benzothiazepin-3(2H)-one (9.8 g, prepared in a similar manner to example 11 of international patent application WO 92/21668) was added to a stirred solution of lithium aluminium hydride (5.01 g) in dry tetrahydrofuran (400 ml). After the addition, the reaction mixture was heated under reflux for five minutes and then cooled. Excess lithium aluminium hydride was decomposed by adding of a saturated aqueous solution of sodium sulphate. The mixture was filtered and the solvent evaporated from the filtrate to give 6-chloro-2,3,4,5-tetrahydro-1,4-benzothiazepine as an oil.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US05580866 |
| Source dataset | uspto-grants-1996_12 |
| ORD ID | ord-cea44638fda74d37bea625e0b91b47d3 |
| Source note | uspto-grants-1996_12 |