反应详情

温度

0 °C

123 ml (1.34 mol) of phosphoryl chloride are added dropwise in the course of 30 minutes at 0° C. to 750 ml of 1,2-dimethoxyethane and 109 ml of dimethyl formamide. The mixture is stirred for a further 30 minutes at 0° C., and, in the course of 45 minutes at 0° C., 180 g (1 mol) of N-(2-(2,5-dimethyl-1H-pyrrolyl)ethyl)acetamide are introduced. After 10 minutes at 0° C., the mixture is allowed to warm to 10° C., stirred for 1 h at 10° C. and hydrolysed by pouring in a solution of 250 g of sodium hydroxide in 920 ml of water in the course of 2 h at 20° C. to the reaction mixture. The resulting reaction mixture is filtered, the organic phase is isolated and the water phase is extracted twice, each time with 370 ml of 1,2-dimethoxyethane. The organic phases are combined and substantially concentrated in vacuum. After addition of 250 ml of toluene, the mixture is concentrated to dehydrate it, 1 l of ethyl acetate is added and the mixture is filtered over silica gel and charcoal, crystallised and dried.

1. waitAfter 10 minutes at 0° C.
2. temperatureto warm to 10° C.
3. stirringstirred for 1 h at 10° C.
4. customThe resulting reaction mixture
5. filtrationis filtered
6. customthe organic phase is isolated
7. extractionthe water phase is extracted twice
8. concentrationsubstantially concentrated in vacuum
9. additionAfter addition of 250 ml of toluene
10. concentrationthe mixture is concentrated
11. additionis added
12. filtrationthe mixture is filtered over silica gel and charcoal
13. customcrystallised
14. customdried