反应详情

To a solution of benzyl trans-4-aminomethylcyclohexylcarbamate hydrochloride (11.56 g), tetrahydro-4H-pyran-4-one (3.85 g), triethylamine (8 ml) and 1,8-diazabicyco[5,4,0]-7-undecene (5.85 g) in 1,2-dichloroethane (100 ml) was added at room temperature sodium triacetoxyborohydride (8.96 g), and the resulting mixture was stirred for 14 hours. To the reaction mixture were added 37% formalin (3.43 g) and sodium triacetoxyborohydride, and the resulting mixture was stirred further for 7 hours. The reaction mixture was mixed with water and was extracted with dichloromethane. The organic layer was washed with an aqueous saturated solution of sodium chloride and was dried with anhydrous magnesium sulfate. After the resulting organic layer was concentrated under reduced pressure, the residue was subjected to separation and purification using column chromatography (ethanol/ethyl acetate 1:4→1:2) to obtain benzyl trans-4-[N-methyl-N-(tetrahydropyran-4-yl)aminomethyl]cyclohexylcarbamate (8.45 g) as colorless crystals.

1. stirringthe resulting mixture was stirred further for 7 hours
2. extractionwas extracted with dichloromethane
3. washThe organic layer was washed with an aqueous saturated solution of sodium chloride
4. dry with materialwas dried with anhydrous magnesium sulfate
5. concentrationAfter the resulting organic layer was concentrated under reduced pressure
6. customthe residue was subjected to separation and purification