HRID2225759
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
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
- temperaturethe mixture was refluxed for 18 hours
- customThe solvents were removed by evaporation
- customthe residue was purified by HPLC (ethyl acetate-methanol-triethylamine; 95:5:2)
- customfollowed by crystallization from ethyl acetate-hexane