HRID492291

反应详情

EQUATION

反应方程式

HRID 492291 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

N′-[(2′-Nitro-1,1′-biphenyl-4-yl)methyl]-N′-pentyl-N-(2,4,6-trifluorophenyl)urea (196.0 mg) and anhydrous tin(II) chloride (401.6 mg) were added to ethanol (4 mL), and the mixture was heated under reflux. One hour later, the solvent was distilled off, and ethyl acetate (15 mL) and a saturated sodium bicarbonate solution (15 mL) were added to the residue. The resultant precipitate was filtered off through Celite. The filtrate was extracted with ethyl acetate. The organic layer was dried over anhydrous sodium sulfate and concentrated under reduced pressure to afford N′-[(2′-amino-1,1′-biphenyl-4-yl)methyl]-N′-pentyl-N-(2,4,6-trifluorophenyl)urea (179.2 mg). Yield: 94%.

WORKUP

后处理

  1. temperaturethe mixture was heated
  2. temperatureunder reflux
  3. distillationOne hour later, the solvent was distilled off
  4. additionethyl acetate (15 mL) and a saturated sodium bicarbonate solution (15 mL) were added to the residue
  5. filtrationThe resultant precipitate was filtered off through Celite
  6. extractionThe filtrate was extracted with ethyl acetate
  7. dry with materialThe organic layer was dried over anhydrous sodium sulfate
  8. concentrationconcentrated under reduced pressure