HRID1823763

反应详情

EQUATION

反应方程式

HRID 1823763 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

15.6 g of 2-amino-5-(4-fluorophenylsulfonyloxy)nitrobenzene were combined with 20.7 g imidazole in 100 ml dimethylformamide in a round bottom flask. The reaction mixture was heated to reflux for 3 hours and then cooled to room temperature. Reaction mixture was then precipitated by addition of water filtered and precipitate was washed with water and dried. Residue was resolubilized in hot ethyl glycol, crystallized by cooling and the crystals were washed with methanol and dried, yielding 10.4 g of 2-amino-5-(4-[1-imidazolyl]-phenylsulfonyloxy)nitro-benzene (melting point 209° C.).

WORKUP

后处理

  1. temperatureThe reaction mixture was heated
  2. temperatureto reflux for 3 hours
  3. customReaction mixture
  4. customwas then precipitated by addition of water
  5. filtrationfiltered
  6. washprecipitate was washed with water
  7. customdried
  8. customcrystallized
  9. temperatureby cooling
  10. washthe crystals were washed with methanol
  11. customdried