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
2-Amino-4-(4-nitrophenoxy)pyridine (600 mg) was dissolved in tetrahydrofuran (12 ml) under a nitrogen atmosphere, and then triethylamine (1.09 ml) and phenyl chloroformate (0.979 ml) were added dropwise thereto, followed by stirring for 20 min. To the reaction mixture was added morpholine (1.81 ml), followed by stirring for 25 min. The reaction mixture was partitioned between ethyl acetate and a saturated aqueous solution of ammonium chloride. The organic layer was washed with a saturated aqueous solution of ammonium chloride, a saturated aqueous solution of sodium hydrogencarbonate, water and brine in this order, and dried over anhydrous sodium sulfate. The solvent was evaporated under a reduced pressure to give a residue, which was then suspended in diethyl ether. The solid was filtered off, and dried under aeration to provide the titled compound (854 mg, 93.8%) as a brown solid.
WORKUP
后处理
- stirringby stirring for 25 min
- customThe reaction mixture was partitioned between ethyl acetate
- washThe organic layer was washed with a saturated aqueous solution of ammonium chloride
- dry with materiala saturated aqueous solution of sodium hydrogencarbonate, water and brine in this order, and dried over anhydrous sodium sulfate
- customThe solvent was evaporated under a reduced pressure
- customto give a residue, which
- filtrationThe solid was filtered off
- customdried under aeration