Reaktion #2122505

Reaktionsgleichung

tert-butyl alcohol

2,5-dihydroxybenzoic acid

sulfuric acid

tert-butyl alcohol

→

salicylic acid

Ausbeute 83.6%

Lösungsmittel

methanol

Reaktionsbedingungen

Aufarbeitung

1. 1
   workup.ADDITIONmixed
2. 2
   SonstigeTo the liquid dispersion obtained
3. 3
   workup.STIRRINGthe mixture was stirred for 30 minutes
4. 4
   SonstigeThe reaction solution obtained
5. 5
   Temperaturwas cooled to room temperature
6. 6
   Sonstigeformed
7. 7
   Filtrationwas filtered
8. 8
   Waschenwhich was then washed with water
9. 9
   Waschenfurther washed with hexane
10. 10
    SonstigeThe precipitate formed
11. 11
    Sonstigethe solution obtained
12. 12
    Sonstigewas re-precipitated in 3.6 L of water
13. 13
    FiltrationAfter filtration
14. 14
    Sonstigethe product was dried at 80° C.

Vorschrift

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).

Quelle