HRID37092
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
CONDITIONS
反应条件
- 温度
- 120 °C
PROCEDURE
实验过程
1.72 g of 5-(2-chloro-5-methoxy-phenoxy)-6-methyl-2-(morpholin-4-yl)-pyrimidin-4-ol were mixed with 3.3 ml of POCl3. The reaction mixture was stirred at 120° C. for 2 hours, thereafter the excess reagent was distilled off. The residue was taken up in chloroform and washed with water, 1N NaOH and water. The organic phase was dried, concentrated and the residue was recrystallized from ether. There were obtained 1.48 g of 4-[4-chloro-5-(2-chloro-5-methoxy-phenoxy)-6-methyl-pyrimidin-2-yl]-morpholine, m.p. 134° C., MS: M=369.
WORKUP
后处理
- distillationthe excess reagent was distilled off
- washwashed with water, 1N NaOH and water
- customThe organic phase was dried
- concentrationconcentrated
- customthe residue was recrystallized from ether