HRID1052919

反应详情

EQUATION

反应方程式

HRID 1052919 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

PROCEDURE

实验过程

A mixed solution of 20 g of 2-bromonitrobenzene, 17 g of 4-chlorophenylboronic acid, 45 g of tripotassium phosphate, 6.9 g of tetrabutylammonium bromide, 480 mg of palladium acetate and 500 ml of dimethylformamide was heated/stirred at 130° C. for 5 hours under a nitrogen flow. The solution was cooled to room temperature, then poured into 100 ml of water, and extracted with 150 ml of toluene. The organic layer was washed with 100 ml of water three times, dried over magnesium sulfate, and then evaporated. The concentrate was purified by silica gel column chromatography and vacuum-dried to obtain 22 g of 2-(4-chlorophenyl)nitrobenzene.

WORKUP

后处理

  1. extractionextracted with 150 ml of toluene
  2. washThe organic layer was washed with 100 ml of water three times
  3. dry with materialdried over magnesium sulfate
  4. customevaporated
  5. customThe concentrate was purified by silica gel column chromatography
  6. customvacuum-dried