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
BOC-Leu-Pro-OBzl (82.76 g, 0.252 mM) was dissolved in methanol (600 ml). 1 N NaOH (327.6 ml, 1.3 molar excess) was added dropwise with ice cooling, and the mixture was stirred for one hour at room temperature. 1 N HCl (6 ml) was added to the reaction mixture with ice cooling, then the methanol was distilled off in vacuo. After washing the water layer with benzene and ethyl acetate, 1 N HCl (260 ml) was added with ice cooling to form an oily material which was extracted with ethyl acetate. The extract was washed with saturated sodium chloride solution and water and dried with anhydrous sodium sulfate. The solution was dried in vacuo and the residue was dissolved in benzene and lyophilized to obtain the substance [11] (58.57 g, yield: 70.8%).
WORKUP
后处理
- distillationthe methanol was distilled off in vacuo
- washAfter washing the water layer with benzene and ethyl acetate, 1 N HCl (260 ml)
- additionwas added with ice cooling
- customto form an oily material which
- extractionwas extracted with ethyl acetate
- washThe extract was washed with saturated sodium chloride solution and water
- dry with materialdried with anhydrous sodium sulfate
- customThe solution was dried in vacuo
- dissolutionthe residue was dissolved in benzene