HRID2225759

反应详情

EQUATION

反应方程式

HRID 2225759 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A solution of 4-[[2-(2-naphthalenyloxy)ethyl]oxy]-alpha-oxobenzeneacetic acid methyl ester (0.5 g) in methanol (75 mL) was treated with N,N-dimethylethylenediamine (0.2 mL) and the mixture was refluxed for 18 hours. The solvents were removed by evaporation and the residue was purified by HPLC (ethyl acetate-methanol-triethylamine; 95:5:2) followed by crystallization from ethyl acetate-hexane to give 0.28 g of N-[2-(dimethylamino)ethyl]-4-[[2-(2-naphthalenyloxy)ethyl]oxy]-alpha-oxobenzeneacetamide as a colorless solid, mp 102°-104° C.

WORKUP

后处理

  1. temperaturethe mixture was refluxed for 18 hours
  2. customThe solvents were removed by evaporation
  3. customthe residue was purified by HPLC (ethyl acetate-methanol-triethylamine; 95:5:2)
  4. customfollowed by crystallization from ethyl acetate-hexane