Reacción #2122505

Ecuación de reacción

tert-butyl alcohol

2,5-dihydroxybenzoic acid

sulfuric acid

tert-butyl alcohol

→

salicylic acid

Rendimiento 83.6%

Disolventes

methanol

Condiciones de reacción

Tratamiento posterior

1. 1
   workup.ADDITIONmixed
2. 2
   OtroTo the liquid dispersion obtained
3. 3
   workup.STIRRINGthe mixture was stirred for 30 minutes
4. 4
   OtroThe reaction solution obtained
5. 5
   Temperaturawas cooled to room temperature
6. 6
   Otroformed
7. 7
   Filtraciónwas filtered
8. 8
   Lavadowhich was then washed with water
9. 9
   Lavadofurther washed with hexane
10. 10
    OtroThe precipitate formed
11. 11
    Otrothe solution obtained
12. 12
    Otrowas re-precipitated in 3.6 L of water
13. 13
    FiltraciónAfter filtration
14. 14
    Otrothe product was dried at 80° C.

Procedimiento

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).

Fuente