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 4-(1-ethyl-propoxy)-6-methyl-N2-(2,4,6-trimethyl-phenyl)-pyridine-2,3-diamine (103 mg, 0.315 mmol) in 4 ml of dry THF was added chloroacetyl chloride (36 mg, 0.315 mmol) and triethylamine (32 mg, 0.315 mmol) at 0° C. The mixture was warmed to room temperature and stirred at room temperature overnight. The mixture was quenched with water and extracted with ethyl acetate. The organic layer was dried and concentrated to give 125 mg of brown residue. The brown residue was purified through silica gel column chromatography using 10% ethyl acetate in hexaneas eluentto give 59 mg of the title compounds as a tan solid, mp 79-82° C. 1H NMR (CDCl3) δ 8.15(brs,1H), 6.87(s,2H), 6.78(s,1H), 6.14(s,1H), 4.20(m,1H), 4.19(s,2H), 2.28(s,3H), 2.24(s,3H), 2.16(s,6H).
WORKUP
后处理
- customThe mixture was quenched with water
- extractionextracted with ethyl acetate
- customThe organic layer was dried
- concentrationconcentrated