HRID1110311

反应详情

EQUATION

反应方程式

HRID 1110311 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

A mixture of 4.0 g (7.67 mmol) of N-[3-hydroxy-5-(octadecyloxy)phenyl]-N-(2-methoxy-2-oxoethyl)glycine methyl ester, 7.8 ml (76.6 mmol) of 1,3-dibromopropane and 5.3 g (38.3 mmol) of potassium carbonate in 75 ml of acetone and 15 ml of DMF was stirred at reflux under argon for 41 hours. The reaction mixture was filtered through a Celite pad and the filtrate was concentrated to a solid which was purified by HPLC using 5% ethyl acetate-toluene to give 3.5 g (72% yield, mp 67°-69°) of N-[3-(3-bromopropoxy)-5-(octadecyloxy)phenyl]-N-(2-methoxy-2-oxoethyl) glycine methyl ester. The structure was confirmed by the nmr spectrum.

WORKUP

后处理

  1. temperatureat reflux under argon for 41 hours
  2. filtrationThe reaction mixture was filtered through a Celite pad
  3. concentrationthe filtrate was concentrated to a solid which
  4. customwas purified by HPLC