HCID 10098451, compound → HCID 11757152, compound

Participants

Reaction Steps

In methanol (10 ml) is dissolved 1-(7,8-dimethoxy-2,3-dihydro-1-benzothiepin-4-carbonyl)-4-(3,4,5-trimethoxybenzoyl)piperazine (1.6 g) obtained in Working Example 24. To the solution is added dropwise, while stirring under ice-cooling, a solution of sodium periodate (960 mg) in water (1 ml). The mixture is stirred for one hour under ice-cooling, and left standing for 48 hours at -5° C. Resultant precipitates are filtered off. To the filtrate is added water, followed by extraction with methylene chloride. The organic layer is washed with an aqueous solution of sodium hydrogencarbonate, dried, and concentrated under reduced pressure. The residue is recrystallized from ethanol-ether to give 1-(7,8-dimethoxy-1-oxo-2,3-dihydro1-benzothiepin-4-carbonyl)-4-(3,4,5-trimethoxybenzoyl)piperazine as colorless prisms (1.3 g), m.p. 138° C.

Provenance & Evidence