HRID1436515

反应详情

EQUATION

反应方程式

HRID 1436515 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

Charge a Schlenck flask with palladium dibenzylidene acetone (88 mg, 0.16 mmol) and tri-o-furyl phosphine (72 mg, 0.31 mmol), purge with nitrogen and add 2 ml of dry THF. Stir until the deep purple solution turns to greenish yellow and add 1-iodo-2-bromobenzene (0.8 ml. 6.2 mmol) followed by 3-methyl-butyl zinc (0.5 M solution in THF, 30 ml, 15 mmol). Stir at room temperature for 4 hours. Add silica gel, concentrate under reduced pressure, load residue onto a flash silica gel column, and elute with hexane to obtain the desired compound as a colorless liquid (1.1 g, 75%).

WORKUP

后处理

  1. custompurge with nitrogen
  2. additionadd 2 ml of dry THF
  3. stirringStir at room temperature for 4 hours
  4. concentrationAdd silica gel, concentrate under reduced pressure, load residue onto a flash silica gel column
  5. washelute with hexane