HRID1452818

反应详情

EQUATION

反应方程式

HRID 1452818 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
5 °C

PROCEDURE

实验过程

To 11.81 g of a toluene solution of (R)-2-bromoisovaleric acid obtained in Example 1 (containing 3.00 g of (R)-2-bromoisovaleric acid), 3.19 g of toluene was further added. After continuously adding 3.00 g of dicyclohexylamine under a nitrogen atmosphere at 5° C. for 1 hour to crystallize. They were successively stirred at 5° C. for 2 hours. The obtained crystals were filtered under a reduced pressure and then the crystals were washed with 3 ml of toluene. The obtained crystals were dried under a reduced pressure to obtain 4.84 g of a (R)-2-bromoisovaleric acid dicyclohexylamine salt (optical purity 99.4% ee, crystallization yield 81%, apparent purity 94.5%, impurity content 2-hydroxy isovaleric acid: 0.04%, bromine content: 3.02%).

WORKUP

后处理

  1. customto crystallize
  2. filtrationThe obtained crystals were filtered under a reduced pressure
  3. washthe crystals were washed with 3 ml of toluene
  4. customThe obtained crystals were dried under a reduced pressure