反应详情

(trans)-N,N-dibenzyl-4-(4-methylpiperazin-1-yl)cyclohexanamine 17a (3.35 g, 8.90 mmol) was dissolved in 20 mL of methanol followed by the addition of palladium/carbon (335 mg, 10%), filled with hydrogen three times. The reaction solution was reacted at 3 atmosphere for 12 hours and filtered. The filtrate was concentrated under reduced pressure followed by the addition of 10 mL of 1 M hydrochloric acid and extracted with dichloromethane (30 mL×3). The aqueous phase was added dropwise with saturated aqueous sodium carbonate solution to adjust pH to 11, extracted with dichloromethane (50 mL×3). The combined organic phase was dried over anhydrous magnesium sulfate, filtered and was concentrated under reduced pressure to obtain the crude title compound (trans)-4-(4-methylpiperazin-1-yl)cyclohexanamine 17b (0.82 g, yield: 46.7%) as a yellow oil liquid, which was used in the next step without further furification.

1. customThe reaction solution was reacted at 3 atmosphere for 12 hours
2. filtrationfiltered
3. concentrationThe filtrate was concentrated under reduced pressure
4. additionfollowed by the addition of 10 mL of 1 M hydrochloric acid
5. extractionextracted with dichloromethane (30 mL×3)
6. additionThe aqueous phase was added dropwise with saturated aqueous sodium carbonate solution
7. extractionextracted with dichloromethane (50 mL×3)
8. dry with materialThe combined organic phase was dried over anhydrous magnesium sulfate
9. filtrationfiltered
10. concentrationwas concentrated under reduced pressure