HRID1973494
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 1.8 g. (6 mmol.) of N-(β,β,β-trichloroethoxycarbonyl)-2-acetoxyglycine n-butyl ester and 1.2 g. (10 mmol.) of 2,6-dimethylphenol in 20 ml. of methylene chloride containing three drops of boron trifluoride etherate was stirred at 25° for 3 hours. The reaction mixture was concentrated in vacuo, 5 ml. of 2:1 hexanemethylene chloride was added and the resulting solution was chromatographed on silica gel. Elution with 2:1 hexanemethylene chloride then with methylene chloride containing increasing amounts of ethyl acetate gave the title compound.
WORKUP
后处理
- concentrationThe reaction mixture was concentrated in vacuo, 5 ml
- additionof 2:1 hexanemethylene chloride was added
- customthe resulting solution was chromatographed on silica gel
- washElution with 2:1 hexanemethylene chloride
- temperaturewith methylene chloride containing increasing amounts of ethyl acetate