HRID1459041

反应详情

EQUATION

反应方程式

HRID 1459041 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
35 °C

PROCEDURE

实验过程

(±)-2-(3-Benzoylphenyl)propionic acid (12.7 g, 50 mmol) was added to MIBK (70 ml) and dissolved with heating to 35° C. Then, (S)-(+)-3-methyl-2-phenylbutylamine (5.24 g, 32 mmol) was added dropwise with stirring. After completing the addition, the reaction solution was stirred at 35° C. to 40° C. for one hour, followed by at room temperature for 5 hours and then at 10° C. for 2 hours. Then, the crystal precipitated was filtered, and the filter cake was washed with cold MIBK (30 ml) and dried to give a diastereomer salt (8.76 g) of (S)-(+)-2-(3-benzoylphenyl)propionic acid with (S)-(+)-3-methyl-2-phenylbutylamine. The yield of the product based on (S)-(+)-2-(3-benzoylphenyl)propionic acid contained in the starting material was 84%.

WORKUP

后处理

  1. dissolutiondissolved
  2. additionthe addition
  3. stirringthe reaction solution was stirred at 35° C. to 40° C. for one hour
  4. waitat 10° C. for 2 hours
  5. customThen, the crystal precipitated
  6. filtrationwas filtered
  7. washthe filter cake was washed with cold MIBK (30 ml)
  8. customdried