反応 #4810

反応方程式

phenol

alpha-methylstyrene

→

2,4-Di-(alpha, alpha-dimethylbenzyl)phenol

溶媒

toluene

反応条件

後処理

1. 1
   温度The reaction mixture is cooled to 110° C.
2. 2
   洗浄After washing the resulting solution at 80° C. with 750 ml of an aqueous solution of 37.5 grams of sodium carbonate and 75 grams of sodium chloride the organic phase
3. 3
   洗浄is washed thrice with 1000 ml of aqueous sodium chloride solution
4. 4
   乾燥then dried over anhydrous sodium sulfate
5. 5
   ろ過filtered
6. 6
   workup.DISTILLATIONvacuum distilled
7. 7
   その他The above-named product is obtained as the main fraction boiling at 172°-175° C./0.15-0.18 mm Hg in a yield of 1229.8 grams (49.6% of theory)

実験手順

This intermediate is made by reacting a mixture of 705.8 grams (7.5 moles) of phenol with 1772.7 grams (15 moles) of alpha-methylstyrene in the presence of 25.7 grams (0.135 moles) of p-toluenesulfonic acid monohydrate catalyst. This mixture is heated under nitrogen at 140° C. for 2.5 hours. The reaction mixture is cooled to 110° C. and 1125 ml of toluene is added. After washing the resulting solution at 80° C. with 750 ml of an aqueous solution of 37.5 grams of sodium carbonate and 75 grams of sodium chloride the organic phase is washed thrice with 1000 ml of aqueous sodium chloride solution; then dried over anhydrous sodium sulfate; filtered and vacuum distilled. The above-named product is obtained as the main fraction boiling at 172°-175° C./0.15-0.18 mm Hg in a yield of 1229.8 grams (49.6% of theory). The product melts at 63°-65° C.

出典