反应详情

0.11 Grams of BF3 -etherate is added to a solution of 2.70 grams of the product from (a) and 4.14 grams of 2,6-di-tert- butyl-4-mercaptophenol dissolved in 30 ml of toluene. The mixture is heated at 55°-65° C. for nine hours and 105°-110° C. for three additional hours. The toluene solution is washed with water and dried over sodium sulfate. The residue, isolated by evaporation of the solvent by distillation in vacuum, is purified by passing a solution in 70:30 heptane:toluene through a flash chromatographic column using silica gel. The isolated residue solidifies on cooling, and melts at 93°-115° C.

1. temperatureThe mixture is heated at 55°-65° C. for nine hours and 105°-110° C. for three additional hours
2. washThe toluene solution is washed with water
3. dry with materialdried over sodium sulfate
4. customThe residue, isolated by evaporation of the solvent by distillation in vacuum
5. customis purified
6. temperatureon cooling