HRID1735363
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
产物
AUXILIARIES
试剂、催化剂与溶剂
PROCEDURE
实验过程
A Grignard compound is prepared from 1.2 g of magnesium, 50 ml of THF and 11.4 g of 4-pentyl-bromobenzene in 25 ml of THF. When the addition is complete, the mixture is refluxed for a further 1 hour and cooled to 10° and 14 g of 4-trifluoromethoxy-bromobenzene in 25 ml of THF and 0.73 g of PdCl2 (dppf) are added. The cooling is removed, but the reaction mixture should not climb above 20°. The mixture is subsequently stirred at room temperature for 16 hours, poured into 100 ml of saturated NH4Cl solution and stirred for a further 15 minutes, and the organic phase is then worked up. After purification by crystallization, trifluoromethoxy-4-(4-pentylphenyl)benzene having C 67° I is obtained.
WORKUP
后处理
- additionWhen the addition
- temperaturethe mixture is refluxed for a further 1 hour
- temperaturecooled to 10°
- customThe cooling is removed
- customclimb above 20°
- additionpoured into 100 ml of saturated NH4Cl solution
- stirringstirred for a further 15 minutes
- customAfter purification
- customby crystallization