HRID1019660
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 194.1 (1044 mg, 7.29 mmol) in EtOH (5207 μL) was added concentrated hydrochloric acid (405 μL, 7.29 mmol). The resulting solution was heated at reflux for 18 hours. The reaction mixture was then cooled to room temperature and poured onto water. The reaction was brought to pH 10 with 1N sodium hydroxide in water and was then extracted with EtOAc. The organic phase was then dried over anhydrous Na2SO4 and filtered to provide ethyl 6-methylpiperidine-3-carboxylate. ESI-MS M+H 172.2.
WORKUP
后处理
- temperatureThe resulting solution was heated
- temperatureat reflux for 18 hours
- additionpoured onto water
- extractionwas then extracted with EtOAc
- dry with materialThe organic phase was then dried over anhydrous Na2SO4
- filtrationfiltered