HRID356647
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
6.55 g of sodium methylate were added at room temperature to a solution of 4-amino-6-chloro-5-(2-methoxy-phenoxy)-2,2'-bipyrimidine in 200 ml of methanol and the solution was subsequently heated at reflux for 32 hours. The methanol was removed on a rotary evaporator, the residue was taken up in methylene chloride and washed with 1N hydrochloric acid. The organic phase was dried over magnesium sulphate, the solvent was finally removed in a water-jet vacuum. The crude product was chromatographed on silica gel with methylene chloride/ methanol (10/1) as the eluent. 4-Amino-6-methoxy-5-(2-methoxy-phenoxy)-2,2'-bipyrimidine was obtained as a lemon-yellow powder MS: 325 (M).
WORKUP
后处理
- temperaturethe solution was subsequently heated
- temperatureat reflux for 32 hours
- customThe methanol was removed on a rotary evaporator
- washwashed with 1N hydrochloric acid
- dry with materialThe organic phase was dried over magnesium sulphate
- customthe solvent was finally removed in a water-jet vacuum
- customThe crude product was chromatographed on silica gel with methylene chloride/ methanol (10/1) as the eluent