HRID492750

反应详情

EQUATION

反应方程式

HRID 492750 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

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

  1. stirringby stirring for 25 min
  2. customThe reaction mixture was partitioned between ethyl acetate
  3. washThe organic layer was washed with a saturated aqueous solution of ammonium chloride
  4. dry with materiala saturated aqueous solution of sodium hydrogencarbonate, water and brine in this order, and dried over anhydrous sodium sulfate
  5. customThe solvent was evaporated under a reduced pressure
  6. customto give a residue, which
  7. filtrationThe solid was filtered off
  8. customdried under aeration