反应详情

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 I 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 a nd 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.

1. additionWhen the addition
2. temperaturethe mixture is refluxed for a further I hour
3. temperaturecooled to 10°
4. customThe cooling is removed
5. customclimb above 20°
6. additionpoured into 100 ml of saturated NH4Cl solution a nd
7. stirringstirred for a further 15 minutes
8. customAfter purification
9. customby crystallization