HRID464779

反应详情

EQUATION

反应方程式

HRID 464779 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

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

  1. temperaturethe solution is heated
  2. washwashed with water
  3. dry with materialThe organic phase is dried over sodium sulfate
  4. concentrationconcentrated
  5. customThe residue is recrystallized from methylene chloride and methanol, there