HRID1170618
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 mixture of N-benzyloxycarbonyl-L-valine (2.50 g, 10.0 mmol), 2,2-dimethyl-1,3-propanediol (5.30 g, 50.9 mmol), dicyclohexylcarbodiimide (2.60 g, 12.6 mmol), and 4-dimethylaminopyridine (125 mg, 1.0 mmol) in 100 mL dry CH2Cl2 was stirred for 23 h. The reaction mixture was filtered and washed successively with 50 mL each of water, saturated aqueous NH4Cl, saturated aqueous NaHCO3, and water. The organic phase was dried over anhydrous Na2SO4 and concentrated. The title compound (2.99 g, 87%) was isolated by flash column chromatography (silica, 2/1 petroleum ether-ethyl acetate) as a white waxy solid.
WORKUP
后处理
- filtrationThe reaction mixture was filtered
- washwashed successively with 50 mL each of water, saturated aqueous NH4Cl, saturated aqueous NaHCO3, and water
- dry with materialThe organic phase was dried over anhydrous Na2SO4
- concentrationconcentrated