반응 #1393

반응 방정식

(1S,2S)-2-dimethylaminomethyl-1-(3-methoxy-phenyl)-cyclohexanol L-(+)-tartrate

caustic soda

→

(1S,2S)-2-dimethylaminomethyl-1-(3-methoxy-phenyl)-cyclohexanol

수율 99.0%

용매

water

반응 조건

후처리

1. 1
   workup.ADDITIONtreated with 900 g
2. 2
   기타crushed ice
3. 3
   추출The mixture was subsequently extracted with 2500 ml dichloromethane
4. 4
   추출was extracted with a further 500 ml dichloromethane
5. 5
   기타after phase separation
6. 6
   건조The combined organic phases were dried over sodium sulphate
7. 7
   기타After removing the solvent
8. 8
   workup.DISTILLATIONby distillation

실험 절차

2050 g (4.95 mole) (1S,2S)-2-dimethylaminomethyl-1-(3-methoxy-phenyl)-cyclohexanol L-(+)-tartrate from step 2 were dissolved in 4000 ml water and treated with 900 g crushed ice. 1000 ml of 36-38% (technical) caustic soda solution were added drop-wise with stirring. The mixture was subsequently extracted with 2500 ml dichloromethane, and was extracted with a further 500 ml dichloromethane after phase separation. The combined organic phases were dried over sodium sulphate. After removing the solvent by distillation, 1280 g (99% theoretical) of (1S,2S)-2-dimethylaminomethyl-1-(3-methoxy-phenyl)-cyclohexanol were obtained as a syrup.

출처