반응 #4810

반응 방정식

phenol

alpha-methylstyrene

→

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

용매

toluene

반응 조건

후처리

1. 1
   온도The reaction mixture is cooled to 110° C.
2. 2
   세척After 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
   세척is washed thrice with 1000 ml of aqueous sodium chloride solution
4. 4
   건조then dried over anhydrous sodium sulfate
5. 5
   여과filtered
6. 6
   workup.DISTILLATIONvacuum distilled
7. 7
   기타The 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)

실험 절차

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.

출처