HRID1612467
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 of t-butyl 2-amino-6-methoxypyridine-4-carboxylate (D55) (0.263 g) and pyridine (0.12 mL) in dichloromethane (16 mL) under argon, was added 4-bromobutyryl chloride (0.17 mL) dropwise (syringe). The reaction was stirred at room temp for 2.5 h and then diluted with ethyl acetate. The mixture was washed with citric acid solution (10% aq.) and the aqueous layer was re-extracted with ethyl acetate. The combined extracts were washed with aq. bicarbonate, water and brine, dried (MgSO4) and evaporated to give the title compound (D56) as a pale yellow gum (0.47 g).
WORKUP
后处理
- washThe mixture was washed with citric acid solution (10% aq.)
- extractionthe aqueous layer was re-extracted with ethyl acetate
- washThe combined extracts were washed with aq. bicarbonate, water and brine
- dry with materialdried (MgSO4)
- customevaporated