HRID26417

反应详情

EQUATION

反应方程式

HRID 26417 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A suspension of 5.2 g. of dimethyl 6-chloro-2,4-pyrimidine-dicarbamate-3-oxide in 300 ml. of methylene chloride is treated with 12.4 g. of 3-hydroxy-piperidine and stirred for 60 hours under an argon atmosphere. The residue is then filtered off and the filtrate is concentrated, a white precipitate separating out. This precipitate is filtered off and recrystallized from a mixture of methylene chloride and methanol, there being obtained pure dimethyl racemic-6-(3-hydroxyl-1-piperidinyl)-2,4-pyrimidine-dicarbamate-3-oxide, having a melting point of 255° C. (decomposition).

WORKUP

后处理

  1. additionA suspension of 5.2 g
  2. filtrationThe residue is then filtered off
  3. concentrationthe filtrate is concentrated
  4. customa white precipitate separating out
  5. filtrationThis precipitate is filtered off
  6. customrecrystallized from a mixture of methylene chloride and methanol, there