反应详情

Ethyl trifluoroacetate (1.31 mL, 11.0 mmol) and triethylamine (1.68 mL, 12.0 mmol) were added to 3-hydroxypiperidine (1.01 g, 10.0 mmol) in ethanol (10 mL). The mixture was stirred at room temperature for 8 hours. Subsequently, the reaction mixture was concentrated and water was added. The mixture was then extracted with ethyl acetate and the extract washed with brine and dried over magnesium sulfate. Purification of the residue by silica gel column chromatography (hexane:ethyl acetate=10:1->2:1) gave 1.68 g (85%) of the desired compound as a colorless oil.

1. concentrationSubsequently, the reaction mixture was concentrated
2. additionwater was added
3. extractionThe mixture was then extracted with ethyl acetate
4. washthe extract washed with brine
5. dry with materialdried over magnesium sulfate
6. customPurification of the residue by silica gel column chromatography (hexane:ethyl acetate=10:1->2:1)