HRID27232

反应详情

EQUATION

反应方程式

HRID 27232 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
45 °C

PROCEDURE

实验过程

2.5 G. of 2-methoxyethyl 2-amino-6-chloro-4-pyrimidinecarbamate-3-oxide are mixed under argon with 3 ml. of 1,2,5,6-tetrahydropyridine and 25 ml. of chloroform. The mixture is stirred at 45° C. for 12 hours, then cooled and washed with 15 ml. of water. The product is extracted with chloroform, the organic phase is dried over sodium sulfate and the solvent is distilled off under reduced pressure. The residue obtained is crystallized from methylene chloride/ether, there being obtained pure 2-methoxyethyl 2-amino-6-[3,6-dihydro-1(2H)-pyridyl]-4-pyrimidinecarbamate having a melting point of 136° C.

WORKUP

后处理

  1. temperaturecooled
  2. washwashed with 15 ml
  3. extractionThe product is extracted with chloroform
  4. dry with materialthe organic phase is dried over sodium sulfate
  5. distillationthe solvent is distilled off under reduced pressure
  6. customThe residue obtained
  7. customis crystallized from methylene chloride/ether, there