反应详情

A mixture of tert-butyl [1-(2-hydroxyethyl)piperidin-4-yl]carbamate (Intermediate 7, 1.7 g, 7 mmol) in dry dichloromethane (20 mL) and triethyl amine (1.4 mL, 9.8 mmol) was treated at 0° C. with methanesulfonyl chloride (0.65 mL, 8.4 mmol). After 45 minutes the reaction was complete by TLC (chloroform/methanol 6:1, rf 0.54). Potassium phosphate buffer (pH 7, 1M, 50 mL) was added, dichloromethane was removed under reduced pressure and it was extracted with ice-cold ethyl acetate (2×100 mL) and dried over sodium sulfate. The solvent was removed under reduced pressure and the crude preparation of the mesylate was used without delay for the next step.

1. customdichloromethane was removed under reduced pressure and it
2. extractionwas extracted with ice-cold ethyl acetate (2×100 mL)
3. dry with materialdried over sodium sulfate
4. customThe solvent was removed under reduced pressure
5. customthe crude preparation of the mesylate