반응 #500806

반응 방정식

sulfuric acid

4′-hydroxy-4-biphenylcarboxylic acid

methanol

methanol

water

→

tan solid

수율 86.0%

Methyl-4′-hydroxy-4-biphenylcarboxylate

수율 86.0%

용매

THF

반응 조건

후처리

1. 1
   온도The reaction mixture was refluxed for three days
2. 2
   기타the solvent was evaporated
3. 3
   여과The resulting solid was filtered
4. 4
   세척washed with water
5. 5
   기타recrystallized
6. 6
   workup.ADDITIONwas added to the solution
7. 7
   workup.ADDITIONwas added
8. 8
   온도After cooling
9. 9
   여과the tan precipitate was filtered
10. 10
    세척washed with cold ethanol, and air
11. 11
    기타dried

실험 절차

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.

출처