HRID2251497

反应详情

EQUATION

反应方程式

HRID 2251497 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture of 5-isopropylpyrimidin-2(1H)-one (2.1 g, 15.2 mmol), POCl3 (15 ml), and N,N-dimethylaniline (5 drops) was heated at reflux under a nitrogen atmosphere for 2 h. Upon cooling, the majority of the POCl3 was removed under reduced pressure. The residue was poured into ice water and extracted with chloroform (3×20 ml). The combined organic extracts were washed with brine, dried over MgSO4 and concentrated to provide 2-chloro-5-isopropylpyrimidine as a light brown oil, which was used without further purification.

WORKUP

后处理

  1. temperaturewas heated
  2. temperatureat reflux under a nitrogen atmosphere for 2 h
  3. temperatureUpon cooling
  4. customthe majority of the POCl3 was removed under reduced pressure
  5. additionThe residue was poured into ice water
  6. extractionextracted with chloroform (3×20 ml)
  7. washThe combined organic extracts were washed with brine
  8. dry with materialdried over MgSO4
  9. concentrationconcentrated