HRID421893

反应详情

EQUATION

反应方程式

HRID 421893 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture of 4-chloro-1,5-dimethyl-6-oxo-2-trimethylsilanylethynyl-1,6-dihydropyridine-3-carboxylic acid ethyl ester (1.00 equivalent), HgSO4 (1.00 equivalent) and H2SO4 (2.00 equivalents) in ˜6:1 acetone:water is refluxed for 3 hours. The reaction mixture is cooled to room temperature and concentrated under reduced pressure. The residue is diluted with a mixture of THF and ethyl acetate and washed with water and brine. The organic layer is dried (MgSO4) and concentrated under reduced pressure. The desired product is obtained by flash column chromatography as necessary.

WORKUP

后处理

  1. concentrationconcentrated under reduced pressure
  2. additionThe residue is diluted with a mixture of THF and ethyl acetate
  3. washwashed with water and brine
  4. dry with materialThe organic layer is dried (MgSO4)
  5. concentrationconcentrated under reduced pressure