反应详情

To 675 ml of toluene were added 20.9 g of 1-[3,5-bis-(1,1-dimethylethyl)-4-hydroxyphenyl]ethanone, 13.3 g of N-dimethylaminorhodanine 6.5 g of ammonium acetate and about 20 ml of acetic acid. The mixture was heated at reflux temperature and any aqueous layer generated was collected in a Dean-Stark trap. Over the following 52 hours an additional 39 g of ammonium acetate and about 100 ml of acetic acid were added in increments and a total of 89.2 ml of aqueous phase was drawn off. Following workup by conventional techniques, 17.1 g of the desired subtitled intermediate was recovered.

1. temperatureThe mixture was heated
2. temperatureat reflux temperature
3. customany aqueous layer generated was collected in a Dean-Stark trap
4. additionOver the following 52 hours an additional 39 g of ammonium acetate and about 100 ml of acetic acid were added in increments
5. customwas recovered