反応 #6292

反応方程式

trifluoroacetophenone

trifluoromethane sulfonic acid

anisole

hydrobromic acid

→

1,1-bis(4-hydroxyphenyl)-1-phenyl-2,2,2-trifluoroethane

溶媒

acetic acid

反応条件

後処理

1. 1
   その他The mixture is then transferred to a separatory funnel
2. 2
   洗浄the organic material is washed with water (3×11), saturated bicarbonate (3×500 ml) and water (2×500 ml)
3. 3
   その他The organic phase is dried
4. 4
   その他the volatiles removed in vacuo
5. 5
   その他The resulting material is crystallized from aqueous methanol
6. 6
   温度The mixture is cooled
7. 7
   workup.ADDITIONpoured
8. 8
   その他over crushed ice
9. 9
   その他the solid collected
10. 10
    その他The crude material is recrystallized from ethanol and petroleum ether

実験手順

A mixture of 100 grams (0.57 mol) of trifluoroacetophenone, 100 grams (0.7 mol) trifluoromethane sulfonic acid, and 100 grams (10.9 mol) anisole is stirred at room temperature for 24 hours. The mixture is then transferred to a separatory funnel and the organic material is washed with water (3×11), saturated bicarbonate (3×500 ml) and water (2×500 ml). The organic phase is dried and the volatiles removed in vacuo. The resulting material is crystallized from aqueous methanol. 37.2 grams (0.1 mol) of this product is refluxed with glacial acetic acid saturated with anhydrous hydrobromic acid. The mixture is cooled and poured over crushed ice and the solid collected. The crude material is recrystallized from ethanol and petroleum ether to give 1,1-bis(4-hydroxyphenyl)-1-phenyl-2,2,2-trifluoroethane.

出典