HRID1912212

反应详情

EQUATION

反应方程式

HRID 1912212 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

Preparation procedure: 3,6-dibromo-o-phenylene diamine (1.0 g, 3.7 mmol) is added to an acetic acid (20 mL) solution of benzil (0.39 g, 1.84 mmol) at 120° C. The resulting solution is mixed homogeneously and reflux for 12 hours. The reaction solution is poured into water, neutralized with sodium bicarbonate, extracted with chloroform, washed with saturated brine water, and dried over anhydrous sodium sulfate. The solvents are removed using a rotary evaporator. The crude product is subjected to column chromatography to give a white solid, which is then recrystallized in chloroform/n-hexane to afford a white solid powder (yield 86%), MALDI-TOF-MS (m/z): 440.1 (M+).

WORKUP

后处理

  1. customPreparation procedure
  2. additionThe resulting solution is mixed homogeneously
  3. temperaturereflux for 12 hours
  4. extractionextracted with chloroform
  5. washwashed with saturated brine water
  6. dry with materialdried over anhydrous sodium sulfate
  7. customThe solvents are removed
  8. customa rotary evaporator
  9. customto give a white solid, which
  10. customis then recrystallized in chloroform/n-hexane