Sodium Sulfate → 2,3,4,5-Tetrahydrobenzo[f][1,4]thiazepine

Participants

Reaction Steps

4,5-Dihydro-1,4-benzothiazepin-3(2H)-one (12 g, prepared in a similar manner to example 1 of international patent application WO 92/21668) was added to a stirred solution of lithium aluminium hydride (6.3 g) in dry tetrahydrofuran (400 ml). After the addition, the reaction mixture was heated under reflux for ten minutes and cooled. Excess of lithium aluminium hydride was decomposed by adding a saturated aqueous solution of sodium sulphate. The mixture was filtered and the solvent was removed from the filtrate by evaporation to give 2,3,4,5-tetrahydro-1,4-benzothiazepine as an oil which was used without further purification. Yield 9.4 g.

Provenance & Evidence