反应详情

To a solution of methyl 2-(3-fluoro-4-(trifluoromethyl)benzyl)piperidine-4-carboxylate (5.96 g, 18.67 mmol) in DCM (100 mL) cooled in an ice-bath was added DIPEA (4 mL, 22.96 mmol) followed by methyl carbonochloridate (1.617 mL, 20.53 mmol). After completed addition the reaction mixture was stirred at room temperature for 2 h. The solvents were evaporated and the residue partitioned between ethyl acetate and 3.8 M HCl. After phase separation the organic layer was washed with brine, then dried over MgSO4 and evaporated. Dimethyl 2-(3-fluoro-4-(trifluoromethyl)benzyl)piperidine-1,4-dicarboxylate (7.17 g, 102%) was isolated as a pale yellow oil.

1. additionaddition the reaction mixture
2. customThe solvents were evaporated
3. customthe residue partitioned between ethyl acetate and 3.8 M HCl
4. customAfter phase separation the organic layer
5. washwas washed with brine
6. dry with materialdried over MgSO4
7. customevaporated