HRID1459039

反应详情

EQUATION

反应方程式

HRID 1459039 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
40 °C

PROCEDURE

实验过程

(±)-2-(3-Benzoylphenyl)propionic acid (20.3 g, 80 mmol) was dissolved in methyl isobutyl ketone (hereinafter abbreviated to "MIBK") (90 g) with heating. Then, (S)-(+)-3-methyl-2-phenylbutylamine (6.68 g, 41 mmol) was added dropwise with stirring at 40° C. After completing the addition, the reaction solution was stirred at 40° C. for one hour and then cooled slowly to 10° C. over 6 hours. After stirring at 10° C. for 3 hours, the precipitated crystal was filtered and the filter cake was washed with cold MIBK (50 ml) and then dried. In this manner, a diastereomer salt (11.5 g) of (S)-(+)-2-(3-benzoylphenyl)propionic acid with (S)-(+)-3-methyl-2-phenylbutylamine was obtained.

WORKUP

后处理

  1. temperaturewith heating
  2. additionthe addition
  3. stirringthe reaction solution was stirred at 40° C. for one hour
  4. temperaturecooled slowly to 10° C. over 6 hours
  5. stirringAfter stirring at 10° C. for 3 hours
  6. filtrationthe precipitated crystal was filtered
  7. washthe filter cake was washed with cold MIBK (50 ml)
  8. customdried