HRID1458667

反应详情

EQUATION

反应方程式

HRID 1458667 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A solution of 7.0 g (20.9 mmol) of 5-methoxycarbonyl-6-ethyl-4-(cis-4-(trimethylsilyl)cyclohexylamino)pyrimidine (Example 6) in 30 ml of absolute tetrahydrofuran was added dropwise to a suspension, cooled to -30° C., of 1.03 g (27.1 mmol) of lithium aluminum hydride in 10 ml of absolute tetrahydrofuran, and the mixture was stirred at room temperature until the end of reaction. Following the hydrolysis, the mixture was subjected to extraction with diethyl ether to give, after drying and removal of the solvent, 6.13 g (19.9 mmol)=95% of the hydroxymethyl compound in the form of white crystals.

WORKUP

后处理

  1. customthe hydrolysis
  2. extractionthe mixture was subjected to extraction with diethyl ether
  3. customto give
  4. customafter drying
  5. customremoval of the solvent, 6.13 g (19.9 mmol)=95% of the hydroxymethyl compound in the form of white crystals