反应详情

温度

47 °C

A solution of 7.5 g (30 mmol) of tungstic acid, 5.2 g (52 mmol) of concentrated sulfuric acid, 32.7 g (200 mmol) of 2,6-dichloroaniline, and 5.84 g (20 mmol) of myristyltrimethylammonium bromide in 74 ml of a toluene was heated to 47° C., and 53 ml (600 mmol) of a 35% hydrogen peroxide solution was added dropwise over 10 hours. The pH value at this time was 0.3. After the completion of the dropwise addition, the mixture was stirred at 47° C. for 4 hours. After the disappearance of the 2,6-dichloroaniline was confirmed by HPLC analysis (area percentage method), 230 ml of toluene and 20 g (160 mmol) of a 25% aqueous sodium hydroxide solution were added. The pH value at this time was 13.5. The reaction liquid was separated at 75° C., and 91 g of the aqueous layer was removed. Then, the obtained organic layer was cooled to 60° C. or less. 35 g (300 mmol) of a 48% aqueous potassium hydroxide solution was added, and 34 ml (400 mmol) of a 35% hydrogen peroxide solution was added dropwise while the reaction temperature was adjusted to 60° C. or less. After the completion of the dropwise addition, the mixture was stirred at 60° C. for 2 hours, and the reaction was completed. The reaction liquid was separated at room temperature. The obtained organic layer was analyzed by gas chromatography by the absolute calibration method, and as a result, the yield was 81%.

1. additionAfter the completion of the dropwise addition
2. additionwere added
3. customThe reaction liquid
4. customwas separated at 75° C.
5. custom91 g of the aqueous layer was removed
6. temperatureThen, the obtained organic layer was cooled to 60° C. or less
7. addition35 g (300 mmol) of a 48% aqueous potassium hydroxide solution was added
8. addition34 ml (400 mmol) of a 35% hydrogen peroxide solution was added dropwise while the reaction temperature
9. customwas adjusted to 60° C. or less
10. additionAfter the completion of the dropwise addition
11. stirringthe mixture was stirred at 60° C. for 2 hours
12. customThe reaction liquid
13. customwas separated at room temperature