反应详情

Methyl trans-4-aminocyclohexanecarboxylate hydrochloride (45.31 g) is suspended in dichloromethane (1000 ml), thereto is added 4-chlorobutyryl chloride (31.5 ml) under ice-cooling and to the mixture is added dropwise a solution of triethylamine (81.5 ml) in dichloromethane (80 ml). The reaction solution is warmed to room temperature, stirred for 3 hours and the reaction solution is concentrated under reduced pressure. To the resulting residue are poured ethyl acetate and 5% hydrochloric acid, and the organic layer is separated, washed with saturated aqueous sodium hydrogen carbonate solution and saturated brine. The organic layer is dried over sodium sulfate and treated with activated carbon, and the filtrate is concentrated under reduced pressure. The resulting residue is suspended in diisopropyl ether, filtered to collect the precipitates, dried to give methyl trans-4-(4-chlorobutyrylamino)cyclohexanecarboxylate (38.81 g).

1. temperaturecooling and to the mixture
2. concentrationthe reaction solution is concentrated under reduced pressure
3. additionTo the resulting residue are poured ethyl acetate and 5% hydrochloric acid
4. customthe organic layer is separated
5. washwashed with saturated aqueous sodium hydrogen carbonate solution and saturated brine
6. dry with materialThe organic layer is dried over sodium sulfate
7. additiontreated with activated carbon
8. concentrationthe filtrate is concentrated under reduced pressure
9. filtrationfiltered
10. customto collect the precipitates
11. customdried