HRID2244025

反应详情

EQUATION

反应方程式

HRID 2244025 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

Add N-bromosuccinimide (9.34 g, 52.5 mmol) and AIBN (5 mg, 0.32 mmol) to a solution of 3-methyl-benzenesulfonyl chloride (10.0 g, 52.5 mmol) in carbon tetrachloride (52 mL), and heat the solution at reflux for 12 hours. Filter the mixture to remove solids and condense under reduced pressure to afford a thick oil. Purify by flash chromatography to yield the title compound as an off-white crystalline solid (5.24 g, 19.4 mmol): 1H NMR (CDCl3) δ 4.54 (s, 2H), 7.62 (m, 1H), 7.78 (m, 1H), 7.98 (m, 1H), 8.06 (m, 1H).

WORKUP

后处理

  1. temperatureheat the solution
  2. temperatureat reflux for 12 hours
  3. filtrationFilter the mixture
  4. customto remove
  5. customsolids and condense under reduced pressure
  6. customto afford a thick oil
  7. customPurify by flash chromatography