反应详情

To a solution of thioether from Example 1, (460 g, 2 moles) and propionyl chloride (202 g, 2.2 moles) in dichloromethane (8 L) at -15° C. was added in portions of approximately 30 g over 1 hour, aluminum chloride (320 g, 2.4 moles). After two hours at -15° C. the reaction mixture was quenched with ice until it became colorless. 1N HCl (2 L) was added and the reaction mixture was stirred until two clear phases were obtained (approximately 30 minutes). The organic layer was siphoned off and dried (Na2SO4). Evaporation afforded an oil which crystallized upon addition of hexane (2 L) and cooling in ice water bath; yield 470 g, m.p. 40°-41° C.

1. customAfter two hours at -15° C. the reaction mixture was quenched with ice until it
2. addition1N HCl (2 L) was added
3. customwere obtained (approximately 30 minutes)
4. dry with materialdried (Na2SO4)
5. customEvaporation
6. customafforded an oil which
7. customcrystallized upon addition of hexane (2 L)
8. temperaturecooling in ice water bath