تفاعل #456709

معادلة التفاعل

sulfuric acid

4'-hydroxy-4-biphenylcarboxylic acid

methanol

methanol

water

→

tan solid

المردود 86.0%

Methyl-4'-hydroxy-4-biphenylcarboxylate

المردود 86.0%

المذيبات

THF

ظروف التفاعل

المعالجة

1. 1
   درجة الحرارةThe reaction mixture was refluxed for three days
2. 2
   أخرىthe solvent was evaporated
3. 3
   ترشيحThe resulting solid was filtered
4. 4
   غسيلwashed with water
5. 5
   أخرىrecrystallized
6. 6
   workup.ADDITIONwas added to the solution
7. 7
   workup.ADDITIONwas added
8. 8
   درجة الحرارةAfter cooling
9. 9
   ترشيحthe tan precipitate was filtered
10. 10
    غسيلwashed with cold ethanol, and air
11. 11
    أخرىdried

الإجراء التجريبي

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.

المصدر