HRID1436515
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
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
- custompurge with nitrogen
- additionadd 2 ml of dry THF
- stirringStir at room temperature for 4 hours
- concentrationAdd silica gel, concentrate under reduced pressure, load residue onto a flash silica gel column
- washelute with hexane