HRID542137
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
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
- temperatureat reflux for 20 hours
- concentrationconcentrated in vacuo
- customThe residue was quenched with water
- extractionextracted with ether
- extractionThe ether extract
- washwas washed successively with 10% K2CO3 and water
- dry with materialdried (CaSO4)
- concentrationconcentrated in vacuo