HRID487345
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 10.1 g of 5 (4-hydroxypiperidino)-2-nitrobenzaldehyde and 34.4 g of ethyl malonate sodium salt in 120 ml of pyridine were added 9.9 g of concentrated sulfuric acid and 850 mg of piperidine. After refluxing for 1 hr, the reaction mixture was concentrated under a reduced pressure. Dilute hydrochloric acid was added to the residue and it was extracted with chloroform. The extract was washed with water, dried, and evaporated under a reduced pressure. The residue was purified by a silica gel column chromatography to give 10.6 g of ethyl 5-(4-hydroxypiperidino)-2-nitrocinnamate.
WORKUP
后处理
- temperatureAfter refluxing for 1 hr
- concentrationthe reaction mixture was concentrated under a reduced pressure
- additionDilute hydrochloric acid was added to the residue and it
- extractionwas extracted with chloroform
- washThe extract was washed with water
- customdried
- customevaporated under a reduced pressure
- customThe residue was purified by a silica gel column chromatography