HRID1936758
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
PROCEDURE
实验过程
6-(5-Trifluoromethyl-1,3,4-oxadiazol-2-yl)quinazolin-4-one (0.79 g) was treated with phosphorus oxychloride (18 ml) and triethylamine (8 ml) at reflux under N2 for 2 hours. The mixture was concentrated in vacuo and the residue azeotroped with toluene. This was then taken up in ethyl acetate and washed with 5% sodium bicarbonate and saturated brine, dried over magnesium sulphate and concentrated in vacuo to give the title compound (0.76 g) as an orange solid; δH CDCl3 9.17(1H,s), 9.05 (1H,d), 8.69(1H,dd), 8.30(1H,d).
WORKUP
后处理
- temperatureat reflux under N2 for 2 hours
- concentrationThe mixture was concentrated in vacuo
- customthe residue azeotroped with toluene
- washwashed with 5% sodium bicarbonate and saturated brine
- dry with materialdried over magnesium sulphate
- concentrationconcentrated in vacuo