HRID730586

反应详情

EQUATION

反应方程式

HRID 730586 的结构方程式

PROCEDURE

实验过程

Potassium carbonate (2.58 g, 18.73 mmol) was added to a solution of 1-bromo-3-fluoro-2-nitro-benzene (2.06 g, 9.36 mmol) and benzylamine (1.13 mL, 9.364 mmol) and the resulting suspension was stirred at room temperature for 18 hours. The reaction mixture was poured onto 500 mL of ice water and extracted four times with 100 mL ethyl acetate. The combined organic fractions were dried over sodium sulfate, and concentrated in vacuo to give an oil that was purified by recrystallization from 75 mL refluxing ethanol with 3 mL water. 1.83 g of benzyl-(3-bromo-2-nitro-phenyl)-amine was collected by filtration as fine red needles. MS: 308, 309 (M+H)+.

WORKUP

后处理

  1. extractionextracted four times with 100 mL ethyl acetate
  2. dry with materialThe combined organic fractions were dried over sodium sulfate
  3. concentrationconcentrated in vacuo
  4. customto give an oil that
  5. customwas purified by recrystallization from 75 mL
  6. temperaturerefluxing ethanol with 3 mL water
  7. filtration1.83 g of benzyl-(3-bromo-2-nitro-phenyl)-amine was collected by filtration as fine red needles