HRID487345

反应详情

EQUATION

反应方程式

HRID 487345 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

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

  1. temperatureAfter refluxing for 1 hr
  2. concentrationthe reaction mixture was concentrated under a reduced pressure
  3. additionDilute hydrochloric acid was added to the residue and it
  4. extractionwas extracted with chloroform
  5. washThe extract was washed with water
  6. customdried
  7. customevaporated under a reduced pressure
  8. customThe residue was purified by a silica gel column chromatography