反应详情

To a suspension of 50 g (0.118 mole) of (Z)-3-ethoxycarbonyl-4-(4-chlorophenyl)-4-(4-methanesulphonylphenyl)-3-butenoic acid, prepared in example 3, in 1000 ml of ethanol is added a solution of 10.4 g (0.26 mole) of sodium hydroxide in 25 ml of water. The mixture is heated under reflux for 6 hours, the precipitate is filtered off and washed with ethanol. The solid is then taken up into 500 ml of a 1N sodium hydroxide solution and the insoluble is filtered off. The aqueous phase is washed with dichloromethane and then acidified with hydrochloric acid to pH=1. After one hour's stirring, the precipitate obtained is filtered under suction, washed with water and dried to give 38.4 g of (Z)-2-[1-(4-chlorophenyl)-1-(4-methanesulphonylphenyl)-methylene]succinic acid in the form of crystals with a melting point of 199-200° C.

1. temperatureThe mixture is heated
2. temperatureunder reflux for 6 hours
3. filtrationthe precipitate is filtered off
4. washwashed with ethanol
5. filtrationthe insoluble is filtered off
6. washThe aqueous phase is washed with dichloromethane
7. customthe precipitate obtained
8. filtrationis filtered under suction
9. washwashed with water
10. customdried