反应详情

温度

65 °C

50 g 2-chloro-N-(2,2-dimethoxy-ethyl)-N-methyl-acetamide in 100 ml n-butyl acetate are added dropwise to a suspension of 35.3 g trans-4-aminocyclohexanol and 53 g potassium carbonate in 150 ml n-butyl acetate at 90-100° C. within 2.5 h. After 45 min the suspension is filtered at 65° C. and washed with 70 ml of n-butyl acetate warmed to 65° C. 100 ml solvent are distilled off from the filtrate and the solution evaporated down is inoculated with product at 40° C. After 16 h at ambient temperature the precipitate is filtered off and washed with 70 ml tert-butylmethylether. After drying, 50 g product is obtained.

1. filtrationAfter 45 min the suspension is filtered at 65° C.
2. washwashed with 70 ml of n-butyl acetate
3. distillation100 ml solvent are distilled off from the filtrate
4. customthe solution evaporated down
5. customis inoculated with product at 40° C
6. filtrationAfter 16 h at ambient temperature the precipitate is filtered off
7. washwashed with 70 ml tert-butylmethylether
8. customAfter drying