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
D-Leucine methyl ester hydrochloride (20 g, 110.43 mmol) is dissolved in methanol. To this is added sodium acetate (22.64 g, 276 mmol) followed by 3-pyridine carboxaldehyde (10.9 mL, 115.5 mmol). The mixture is allowed to stir at room temperature for 15 minutes and then sodium cyanoborohydride (4.15 g, 66 mmol) is added slowly over 15 minutes. After stirring for 16 hours at room temperature methanol is evaporated under reduced pressure and the resulting oil is taken up in ethyl acetate and washed with water (2×). The organics are dried over sodium sulfate and concentrated to an oil. The product is purified by silica gel flash chromatography (100% ethyl acetate) to give N-(3-picolyl) D-leucine methyl ester as an oil.
WORKUP
后处理
- customis evaporated under reduced pressure
- washwashed with water (2×)
- dry with materialThe organics are dried over sodium sulfate
- concentrationconcentrated to an oil
- customThe product is purified by silica gel flash chromatography (100% ethyl acetate)