HRID1110256

反应详情

EQUATION

反应方程式

HRID 1110256 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A solution of 2.0 g (3.3 mmol) of N-(carboxymethyl)-N-[3-(octadecyloxy)-5-[(5-methoxy-5-oxopentyl)oxy]phenyl]glycine and 2.8 ml (16.5 mmol) of 6N NaOH in 100 ml of methanol was stirred at reflux under argon for 16 hours. After cooling to room temperature, the precipitated sodium salt was removed by filtration, dissolved in 300 ml of water and the mixture was acidified with 4 ml of 6N HCl. The product was extracted with ethyl acetate and the dried extract was concentrated at reduced pressure to a solid which was recrystallized from acetone-hexane to give 1.8 g (92% yield, mp 126°-128°) of N-[3-(4-carboxybutoxy)-5-(octadecyloxy)phenyl]-N-(carboxymethyl)glycine.

WORKUP

后处理

  1. temperatureat reflux under argon for 16 hours
  2. customthe precipitated sodium salt was removed by filtration
  3. dissolutiondissolved in 300 ml of water
  4. extractionThe product was extracted with ethyl acetate
  5. extractionthe dried extract
  6. concentrationwas concentrated at reduced pressure to a solid which
  7. customwas recrystallized from acetone-hexane