HRID1729160
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
A mixture of 1.5 g of 7-[(4,6-dimethoxy-pyrimidin-2-yl)oxy]-3-hydroxy-phthalide (see Example 84) and 2.5 g of (ethoxycarbonylmethylene)-triphenyl-phosphorane is maintained at reflux temperature for 10 hours in approximately 40 ml of tetrahydrofuran. The solvent is then evaporated off and the reaction material which remains is purified on a column of silica gel (eluant: ethyl acetate/n-hexane 1:1) to yield 3-(ethoxycarbonylmethyl)-7-[(4,6-dimethoxy-pyrimidin-2-yl)oxy]-phthalide, m.p. 150°-152° C.
WORKUP
后处理
- temperatureis maintained
- customThe solvent is then evaporated off
- customthe reaction material which remains is purified on a column of silica gel (eluant: ethyl acetate/n-hexane 1:1)