反应详情

109 g of mesyl chloride in 250 ml THF are added dropwise to 150 g (trans)-1-hydroxy-4-(4-methyl-3-oxo-piperazin-1-yl)-cyclohexane and 162 ml triethylamine in 2300 ml THF in such a way that the temperature does not exceed 35° C. After 25 min the suspension is filtered and washed with 300 ml THF. The filtrate is evaporated down in vacuo at 40° C. to a total mass of 520 g. 230 ml ethyl acetate are added to the suspension. After 15 min the mixture is filtered and the precipitate is washed with 230 ml of ethyl acetate and 150 ml of methyl-tert-butyl ether. After drying, 153.1 g product are obtained.

1. customdoes not exceed 35° C
2. filtrationAfter 25 min the suspension is filtered
3. washwashed with 300 ml THF
4. customThe filtrate is evaporated down in vacuo at 40° C. to a total mass of 520 g
5. addition230 ml ethyl acetate are added to the suspension
6. filtrationAfter 15 min the mixture is filtered
7. washthe precipitate is washed with 230 ml of ethyl acetate and 150 ml of methyl-tert-butyl ether
8. customAfter drying