HRID488335

反应详情

EQUATION

反应方程式

HRID 488335 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture of 1.3 g (2.17 mmol) of N-(2-ethoxy-2-oxoethyl)-N-[1,2-dioxo-2-[4-[(12-phenoxydodecyl)oxy]phenyl]ethyl]glycine ethyl ester and 1.8 ml (10.8 mmol) of 6N NaOH in 125 ml of methanol was stirred at reflux for 3.5 hours. The reaction mixture was cooled in an ice bath and the precipitated sodium salt was filtered. The sodium salt was suspended in water, acidified with 6N HCl and extracted with ethyl acetate. The dried extract was concentrated to a solid which was triturated with hexane and filtered to give 1.04 g (88% yield, mp 130°-132°) of N-(carboxymethyl)-N-[1,2-dioxo-2-[4-[(12-phenoxydodecyl)oxy]phenyl]ethyl]glycine.

WORKUP

后处理

  1. temperatureat reflux for 3.5 hours
  2. temperatureThe reaction mixture was cooled in an ice bath
  3. filtrationthe precipitated sodium salt was filtered
  4. extractionextracted with ethyl acetate
  5. extractionThe dried extract
  6. concentrationwas concentrated to a solid which
  7. customwas triturated with hexane
  8. filtrationfiltered