反应详情

温度

50 °C

A 50 L flask was set up with a mechanical stirrer, inlet for inert atmosphere, and cooling capacity. The flask was placed under an argon atmosphere and was charged with 2961.5 g (16.2 moles) of R-131 and 9.0 L of THF. The flask was cooled on ice to less than 5° C. Thionyl chloride (1200 mL, 16.4 moles) dissolved in 6.0 L of THF was added slowly via an addition funnel to the reaction flask. The temperature of the reaction flask was maintained less than or equal to 10° C. The addition time was 1 hour 10 minutes. The reaction mixture was allowed to agitate for an additional 2 hours 50 minutes. Then a solution of 2359.4 g of (11.4 moles) of 4-nitro-3-trifluoromethylaniline (Aldrich, 98%) and 3.83 L of triethylamine in 6.0 L THF was added over a period of 3 hours 5 minutes. The temperature of the reaction flask was maintained less than or equal to 10° C. The ice bath was removed, and the reaction mixture was allowed to stir for 30 minutes. With a heating mantle, the reaction mixture was heated to 50° C. for 15 hours and 10 minutes. After the reaction was complete as analyzed by TLC, the reaction mixture was cooled to less than 30° C. and 7.5 L of deionized water was added. The aqueous layer was removed and a second water wash (7.5 L) was performed. The organic layer was then washed three times with 10% bicarbonate (8.1 L) until the pH was greater than 7.

1. customA 50 L flask was set up with a mechanical stirrer, inlet for inert atmosphere
2. temperaturecooling capacity
3. temperatureThe flask was cooled on ice to less than 5° C
4. additionwas added slowly via an addition funnel to the reaction flask
5. temperatureThe temperature of the reaction flask was maintained less than or equal to 10° C
6. temperatureThe temperature of the reaction flask was maintained less than or equal to 10° C
7. customThe ice bath was removed
8. stirringto stir for 30 minutes
9. temperaturethe reaction mixture was cooled to less than 30° C.
10. addition7.5 L of deionized water was added
11. customThe aqueous layer was removed
12. washa second water wash (7.5 L)
13. washThe organic layer was then washed three times with 10% bicarbonate (8.1 L) until the pH was greater than 7