반응 #2122505

반응 방정식

tert-butyl alcohol

2,5-dihydroxybenzoic acid

sulfuric acid

tert-butyl alcohol

→

salicylic acid

수율 83.6%

용매

methanol

반응 조건

후처리

1. 1
   workup.ADDITIONmixed
2. 2
   기타To the liquid dispersion obtained
3. 3
   workup.STIRRINGthe mixture was stirred for 30 minutes
4. 4
   기타The reaction solution obtained
5. 5
   온도was cooled to room temperature
6. 6
   기타formed
7. 7
   여과was filtered
8. 8
   세척which was then washed with water
9. 9
   세척further washed with hexane
10. 10
    기타The precipitate formed
11. 11
    기타the solution obtained
12. 12
    기타was re-precipitated in 3.6 L of water
13. 13
    여과After filtration
14. 14
    기타the product was dried at 80° C.

실험 절차

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).

출처