反应详情

A solution of 3,4,5-trimethoxybenzoyl chloride (10.9 g) in dichloromethane (100 ml) is added dropwise taking one hour, under ice-cooling while stirring, to a mixture of methyl piperazine-2-carboxylate dihydrochloride (10.24 g), triethylamine (18.7 g) and dichloromethane (200 ml). The reaction mixture is poured into ice-water, followed by extraction with dichloromethane. The organic layer is washed with water, dried and the solvent is distilled off under reduced pressure. Crystals obtained from the residue are recrystallized from ethyl acetate and hexane to afford methyl 4-(3,4,5-trimethoxybenzoyl)piperazine-2-carboxylate (9.6 g) as colorless needles, m.p. 113-114° C.

1. temperaturecooling
2. extractionfollowed by extraction with dichloromethane
3. washThe organic layer is washed with water
4. customdried
5. distillationthe solvent is distilled off under reduced pressure
6. customCrystals obtained from the residue
7. customare recrystallized from ethyl acetate and hexane