反応 #2122505

反応方程式

tert-butyl alcohol

2,5-dihydroxybenzoic acid

sulfuric acid

tert-butyl alcohol

→

salicylic acid

収率 83.6%

溶媒

methanol

反応条件

後処理

1. 1
   workup.ADDITIONmixed
2. 2
   その他To the liquid dispersion obtained
3. 3
   workup.STIRRINGthe mixture was stirred for 30 minutes
4. 4
   その他The reaction solution obtained
5. 5
   温度was cooled to room temperature
6. 6
   その他formed
7. 7
   ろ過was filtered
8. 8
   洗浄which was then washed with water
9. 9
   洗浄further washed with hexane
10. 10
    その他The precipitate formed
11. 11
    その他the solution obtained
12. 12
    その他was re-precipitated in 3.6 L of water
13. 13
    ろ過After filtration
14. 14
    その他the product was dried at 80° C.

実験手順

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).

出典