反应详情

40 g (0.0938 mole) of α-chloro-N,N-dimethyl-2-(5-methylthien-2-yl)imidazo[2,1-b]benzothiazole-3-acetamide hydrochloride in solution in 1200 ml of dichloromethane are treated with 43.6 (0.283 mole) of Rongalite®, while stirring the mixture at room temperature for 6 h. The suspension is filtered, it is rinsed with dichloromethane and the organic phase is washed (pH=1) with 500 ml of 0.5N sodium hydroxide up to a pH>10, then to neutral pH with a saturated sodium chloride solution. The organic phase is dried over sodium sulphate and the solvent is evaporated under reduced pressure. A beige-coloured solid is obtained which is purified by chromatography on a silica gel column, eluting with a 95/5 mixture of dichloromethane/methanol. 23.9 g of a white solid are obtained. Melting point: 216°-218° C.

1. filtrationThe suspension is filtered
2. washit is rinsed with dichloromethane
3. washthe organic phase is washed (pH=1) with 500 ml of 0.5N sodium hydroxide up to a pH>10
4. dry with materialThe organic phase is dried over sodium sulphate
5. customthe solvent is evaporated under reduced pressure
6. customA beige-coloured solid is obtained which
7. customis purified by chromatography on a silica gel column
8. washeluting with a 95/5 mixture of dichloromethane/methanol