HRID968026

反应详情

EQUATION

反应方程式

HRID 968026 的结构方程式

PROCEDURE

实验过程

A mixture of 2,4-dihydroxy-3,6-dimethylpyridine (2.86 g, 20.58 mmol), POCl3 (15 ml) and N,N-dimethylaniline (3.6 ml, 22.64 mmol) was heated at reflux for 3 hours. The mixture was cooled, poured into ice water and extracted with diethyl ether. The organic layer was dried and concentrated to give 3.02 g of the crude material. After silica gel column chromatography using chloroform as eluent, 1.3102 g of the title compound was obtained as a yellow oil. 1H NMR (CDCl3) δ 7.07 (s, 1H), 2.43 (s, 3H), 2.39 (s, 3H) ppm.

WORKUP

后处理

  1. temperaturewas heated
  2. temperatureat reflux for 3 hours
  3. temperatureThe mixture was cooled
  4. extractionextracted with diethyl ether
  5. customThe organic layer was dried
  6. concentrationconcentrated
  7. customto give 3.02 g of the crude material