HRID400455
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
6.7 g potassium carbonate was added to 7 g 5-oxo-azepane-1,4-dicarboxylic acid 1-tert-butyl ester 4-ethyl ester in 50 mL DMF and stirred at RT. After 30 min 6.1 g ethyl bromoacetate was added and the reaction was stirred at RT over night. The reaction was diluted with water and extracted with ethyl acetate/hexane (1/1). The organic phase was washed with brine, dried and concentrated. The residue was purified by column chromatography on silica gel (15% ethyl acetate in hexane) to give 5.6 g of the desired product.
WORKUP
后处理
- stirringthe reaction was stirred at RT over night
- extractionextracted with ethyl acetate/hexane (1/1)
- washThe organic phase was washed with brine
- customdried
- concentrationconcentrated
- customThe residue was purified by column chromatography on silica gel (15% ethyl acetate in hexane)