HRID542137

反应详情

EQUATION

反应方程式

HRID 542137 的结构方程式

PROCEDURE

实验过程

A mixture of 5.0 g (0.016 mol) of product of Example 35, 4.52 g (0.0362 mol) of 2,6-lutidine and 34 ml of phosphorus oxychloride was held at reflux for 20 hours and concentrated in vacuo. The residue was quenched with water and extracted with ether. The ether extract was washed successively with 10% K2CO3 and water, dried (CaSO4) and concentrated in vacuo to give 3.06 g (57.8%) of product as a brown oil, nD25 1.4313.

WORKUP

后处理

  1. temperatureat reflux for 20 hours
  2. concentrationconcentrated in vacuo
  3. customThe residue was quenched with water
  4. extractionextracted with ether
  5. extractionThe ether extract
  6. washwas washed successively with 10% K2CO3 and water
  7. dry with materialdried (CaSO4)
  8. concentrationconcentrated in vacuo