HRID1496650

反应详情

EQUATION

反应方程式

HRID 1496650 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

PROCEDURE

实验过程

To a mixture of 2-chloro-5-iodotoluene (4.07 g, 16.12 mmol), N-bromosuccinimide (3.16 g, 17.73 mmol) in dichloromethane (258 mL) and water (258 mL) was added 2,2′-azodiisobutyronitrile (0.132 g, 0.81 mmol). The reaction mixture was irradiated with a halogen sun lamp (150 watt) for 2 h and then cooled to room temperature. The two-phase reaction mixture was separated, and the aqueous layer was extracted with dichloromethane (50 mL). The combined organic layers were washed with water (2×150 mL), dried over magnesium sulfate, filtered and concentrated under reduced pressure to provide the title compound as an orange oil (5.20 g).

WORKUP

后处理

  1. customThe reaction mixture was irradiated with a halogen sun lamp (150 watt) for 2 h
  2. customThe two-phase reaction mixture
  3. customwas separated
  4. extractionthe aqueous layer was extracted with dichloromethane (50 mL)
  5. washThe combined organic layers were washed with water (2×150 mL)
  6. dry with materialdried over magnesium sulfate
  7. filtrationfiltered
  8. concentrationconcentrated under reduced pressure