反应详情

3 kg (10 mole) (1RS,2RS)-2-dimethylaminomethyl-1-(3-methoxy-phenyl)-cyclohexanol hydrochloride (1) were suspended in 4800 ml water and treated with 1.6 kg crushed ice. 1300 ml of 36-38% (technical) caustic soda solution were added drop-wise with stirring. The mixture was subsequently extracted with 7000 ml dichloromethane, and was extracted with a further 2000 ml dichloromethane after phase separation. The combined organic phases were dried over sodium sulphate. After removing the solvent by distillation, 2630 g (99% theoretical) of (1RS,2RS)-2-dimethylaminomethyl-1-(3-methoxy-phenyl)-cyclohexanol were obtained as a syrup.

1. additiontreated with 1.6 kg
2. customcrushed ice
3. extractionThe mixture was subsequently extracted with 7000 ml dichloromethane
4. extractionwas extracted with a further 2000 ml dichloromethane
5. customafter phase separation
6. dry with materialThe combined organic phases were dried over sodium sulphate
7. customAfter removing the solvent
8. distillationby distillation