HRID1712243
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
The suspension of 1.79 g of 6-hydroxymethyl-4H-benzo[1,4]oxazin-3-one, 2.20 ml of 1-chloro-3-methoxypropane, 10 g of KF on alumina and 0.033 g of potassium iodide in 150 ml of acetonitrile is stirred at reflux over 72 hours. The reaction mixture is cooled and clarified by filtration, and the filtrate is concentrated by evaporation to dryness. The title compound is obtained from the residue by means of flash chromatography (SiO2 60F). Rf=0.60 (9:1 dichloromethane-methanol); Rt=2.74.
WORKUP
后处理
- temperatureat reflux over 72 hours
- temperatureThe reaction mixture is cooled
- filtrationclarified by filtration
- concentrationthe filtrate is concentrated by evaporation to dryness