HRID1266574

反应详情

EQUATION

反应方程式

HRID 1266574 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
60 °C

PROCEDURE

实验过程

L-AzeOH-D-tartrate (14.0 g; 56 mmol; prepared analogously to the methods described in international patent application WO 97/02441) was added to water (17 mL) at room temperature. The mixture was heated to 60° C. and an additional amount of water (9 mL) was added to completely dissolve the L-AzeOH-D-tartrate. KOH (10.8 mL; 5.7 M) was added over 7 minutes to resultant the yellowish solution. The reaction mixture was then left to cool at room temperature. It was left at this temperature overnight. The reaction mixture was then cooled on ice for 7 h. Potassium hydrogen tartrate crystallised and was filtered off. The filtration gave potassium hydrogen tartrate as white solid (9.5 g; 91%) and a slightly yellowish aqueous solution containing liberated L-AzeOH. The latter was used in the next step without further characterisation.

WORKUP

后处理

  1. customprepared analogously to the methods
  2. waitThe reaction mixture was then left
  3. temperatureto cool at room temperature
  4. temperatureThe reaction mixture was then cooled on ice for 7 h
  5. customPotassium hydrogen tartrate crystallised
  6. filtrationwas filtered off
  7. filtrationThe filtration