HRID464779
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
1.0 g of dimethyl 6-[(p-tolylsulfonyl)oxy]-2,4-pyrimidinedicarbamate-3-oxide is dissolved in 20 ml of chloroform and the solution is heated at reflux with 1 ml of 1,2,5,6-tetrahydropyridine. The cooled mixture is diluted with methylene chloride and washed with water. The organic phase is dried over sodium sulfate and concentrated. The residue is recrystallized from methylene chloride and methanol, there being obtained pure dimethyl 6-[3,6-dihydro-1(2H)-pyridyl]-2,4-pyrimidinedicarbamate-3-oxide of melting point 185°-187°.
WORKUP
后处理
- temperaturethe solution is heated
- washwashed with water
- dry with materialThe organic phase is dried over sodium sulfate
- concentrationconcentrated
- customThe residue is recrystallized from methylene chloride and methanol, there