反应 #2122505

反应方程式

tert-butyl alcohol

2,5-dihydroxybenzoic acid

sulfuric acid

tert-butyl alcohol

→

salicylic acid

收率 83.6%

溶剂

methanol

反应条件

后处理

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

实验过程

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).

来源