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
To a solution containing 60 g (0.30 mol) of N-cyclopentylglycine t- butyl ester and 75 ml (0.54 mol) of triethylamine in 200 ml of methylene chloride at 0° C. was added dropwise a solution of 54 g (0.30 mol) of 3-acetylthio-2-methylpropanoyl chloride in 250 ml of methylene chloride. After the reaction mixture was stirred at room temperature overnight, it was filtered and concentrated in vacuo. The residue was taken up in ethyl acetate and wasned once with saturated aqueous NaHCO3, once with brine, three times with 5% aqueous HCl, once with brine, and five times with saturated aqueous NaHCO3. The organic phase was dried over MgSO4, filtered, and concentrated in vacuo to yield 80.1 g (78%) of N-(3-acetylthio-2-methylpropanoyl)-N-cyclopentylglycine t-butyl ester as an oil which crystallized on standing.
WORKUP
后处理
- filtrationit was filtered
- concentrationconcentrated in vacuo
- dry with materialThe organic phase was dried over MgSO4
- filtrationfiltered
- concentrationconcentrated in vacuo