HRID1912212
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
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
- customPreparation procedure
- additionThe resulting solution is mixed homogeneously
- temperaturereflux for 12 hours
- extractionextracted with chloroform
- washwashed with saturated brine water
- dry with materialdried over anhydrous sodium sulfate
- customThe solvents are removed
- customa rotary evaporator
- customto give a white solid, which
- customis then recrystallized in chloroform/n-hexane