HRID1399822

反应详情

EQUATION

反应方程式

HRID 1399822 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

CONDITIONS

反应条件

温度
60 °C

PROCEDURE

实验过程

To a solution of 5-bromo-N-(4-methoxybenzyl)-2-nitroaniline (750 mg, crude) in EtOH (8 mL) and H2O (8 mL) was added Fe powder (766 mg, 13.7 mmol) and ammonium chloride (733 mg, 13.7 mmol). The mixture was stirred at 60° C. for 4 h then filtered and the filtrate was concentrated to remove EtOH. The residue was then diluted with water and extracted with EtOAc. The organic layer was concentrated to give the desired product (550 mg, crude, 82% yield) with the crude product being used in next step without further purification. LCMS (m/z): 308.1 [M+H]+

WORKUP

后处理

  1. filtrationthen filtered
  2. concentrationthe filtrate was concentrated
  3. customto remove EtOH
  4. additionThe residue was then diluted with water
  5. extractionextracted with EtOAc
  6. concentrationThe organic layer was concentrated