HRID1796206
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
PROCEDURE
实验过程
To a solution of 1-t-butoxycarbonyl-4-hydroxypiperidine (1.45 g), 2-trifluoromethyl-4-nitrophenol (1.38 g), which was prepared from 3-trifluoromethylnitrobenzene according to the method described in J. Org. Chem., 63, 4199 (1998), and triphenylphosphine (2.27 g) in dichloromethane (65 ml), diethyl azodicarboxylate (1.4 ml) was added dropwise with stirring under ice-cooling, and the resulting mixture was stirred at room temperature overnight and then evaporated in vacuo. The residue obtained was purified by chromatography on a silica gel column using dichloromethane as the eluent to afford the title compound (2.28 g, yield: 88%) as a pale yellow oil.
WORKUP
后处理
- temperaturecooling
- stirringthe resulting mixture was stirred at room temperature overnight
- customevaporated in vacuo
- customThe residue obtained
- customwas purified by chromatography on a silica gel column