反应详情

Concentrated sulfuric acid (approximately 4 ml) was carefully added to a solution of 4'-hydroxy-4-biphenylcarboxylic acid (Aldrich) (8.20 g, 38.3 mmol) in 1 liter of methanol. The reaction mixture was refluxed for three days and the solvent was evaporated. The resulting solid was filtered, washed with water, and recrystallized as follows. The crude solid was dissolved in a minimum amount of hot THF, and approximately three equivalents of methanol was added to the solution. The solution was brought to a boil, and water was added with vigorous stirring until the solution remained cloudy. After cooling, the tan precipitate was filtered, washed with cold ethanol, and air dried to yield 7.57 g (86%) of a tan solid.

1. temperatureThe reaction mixture was refluxed for three days
2. customthe solvent was evaporated
3. filtrationThe resulting solid was filtered
4. washwashed with water
5. customrecrystallized
6. additionwas added to the solution
7. additionwas added
8. temperatureAfter cooling
9. filtrationthe tan precipitate was filtered
10. washwashed with cold ethanol, and air
11. customdried