反应详情

A mixture of 9.4 g 1-benzyl-4-hydroxy-piperidine-4-carboxylic acid, hydrochloride, 3.62 g (35 mmol) acetic anhydride, 11.89 mL pyridine in 40 mL DCM was stirred for 1 h at room temperature. KHSO4 (10%) and ethanol were added and filtered. The filtrate was evaporated and the residue was purified by preparative HPLC on reversed phase eluting with a gradient formed from acetonitrile, water and HCOOH. The product containing fractions were evaporated to yield 4.2 g (52%) of the title compound as light yellow solid. MS (m/e): 278.1 [(M+H)+].

1. filtrationfiltered
2. customThe filtrate was evaporated
3. customthe residue was purified by preparative HPLC on reversed phase
4. washeluting with a gradient
5. customformed from acetonitrile, water and HCOOH
6. additionThe product containing fractions
7. customwere evaporated