HRID904894

反应详情

EQUATION

反应方程式

HRID 904894 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

PROCEDURE

实验过程

A solution of methyl N-(3-cyano-4,6-dimethyl-2-pyridyl)-N-(2-dimethylaminoethyl)carbamate (14.8 g, 53 mmol) in glacial acetic (200 ml) containing platinum oxide catalyst (1.1 g) is hydrogenated in a Parr apparatus until two equivalents of hydrogen are taken up (20 hours). The catalyst is removed by filtration and the solvent evaporated to give a residue which is dissolved in water, made basic with sodium carbonate, and the crude product extracted into methylene chloride. This dried solution is evaporated to give a crude product (12.5 g) which is crystallized from cyclohexane to yield 7.2 g of pure title C product; m.p.: 139°-141° C.

WORKUP

后处理

  1. custom(20 hours)
  2. customThe catalyst is removed by filtration
  3. customthe solvent evaporated
  4. customto give a residue which
  5. extractionthe crude product extracted into methylene chloride
  6. customThis dried solution is evaporated