تفاعل #2122505

معادلة التفاعل

tert-butyl alcohol

2,5-dihydroxybenzoic acid

sulfuric acid

tert-butyl alcohol

→

salicylic acid

المردود 83.6%

المذيبات

methanol

ظروف التفاعل

المعالجة

1. 1
   workup.ADDITIONmixed
2. 2
   أخرىTo the liquid dispersion obtained
3. 3
   workup.STIRRINGthe mixture was stirred for 30 minutes
4. 4
   أخرىThe reaction solution obtained
5. 5
   درجة الحرارةwas cooled to room temperature
6. 6
   أخرىformed
7. 7
   ترشيحwas filtered
8. 8
   غسيلwhich was then washed with water
9. 9
   غسيلfurther washed with hexane
10. 10
    أخرىThe precipitate formed
11. 11
    أخرىthe solution obtained
12. 12
    أخرىwas re-precipitated in 3.6 L of water
13. 13
    ترشيحAfter filtration
14. 14
    أخرىthe product was dried at 80° C.

الإجراء التجريبي

100 g of 2,5-dihydroxybenzoic acid and 1,441 g of 80% sulfuric acid were heated to 50° C. and mixed. To the liquid dispersion obtained, 144 g of tert-butyl alcohol was added, and the mixture was stirred at 50° C. for 30 minutes. Thereafter, the operation that 144 g of tert-butyl alcohol was added to the liquid dispersion and the mixture was stirred for 30 minutes was carried out three times. The reaction solution obtained was cooled to room temperature, and then dropwise added to 1 kg of ice water, where the precipitate formed was filtered, which was then washed with water and further washed with hexane. The precipitate formed was dissolved in 200 mL of methanol, and the solution obtained was re-precipitated in 3.6 L of water. After filtration, the product was dried at 80° C. to obtain 74.9 g of a salicylic acid intermediate represented by the following formula (3).

المصدر