反応 #46940

反応方程式

sulfuric acid

tetrafluoroisopthalonitrile

water

sulfuric acid

→

tetrafluoroisophthalamide

収率 98.9%

反応条件

後処理

1. 1
   温度kept cooled
2. 2
   workup.ADDITIONwas added piece meal to the cooled solution
3. 3
   workup.ADDITIONAfter completion of this addition
4. 4
   workup.STIRRINGthe reaction solution in the flask was stirred for one hour while the inner temperature of the flask
5. 5
   その他was kept at 90 to 100° C.
6. 6
   その他from exceeding 60° C
7. 7
   workup.ADDITIONAfter the completion of the dropwise addition
8. 8
   温度the mixture was cooled to 20° C.
9. 9
   その他A white solid which was precipitated
10. 10
    その他was separated by filtration
11. 11
    洗浄washed with 1000 g of water
12. 12
    その他dried

実験手順

In a three neck flask having an inner volume of 1 liter, 63.08 g of purified water and 1048.74 g of 98% sulfuric acid were placed and stirred to prepare a 92% sulfuric acid solution. The resultant solution was heated to 80° C. and then kept cooled to keep the inner temperature of the flask in the range of 90 to 100° C. and 350.13 g (1.75 mols) of tetrafluoroisopthalonitrile was added piece meal to the cooled solution. After completion of this addition, the reaction solution in the flask was stirred for one hour while the inner temperature of the flask was kept at 90 to 100° C. and then the reaction solution was cooled to 30° C. Then, 1400 g of ice was placed in a beaker having an inner volume of 3 liters and the reaction solution was gently added dropwise to the ice so as to keep the inner temperature of the beaker from exceeding 60° C. After the completion of the dropwise addition, the mixture was cooled to 20° C. and then kept at 20° C. for one hour. A white solid which was precipitated was separated by filtration, washed with 1000 g of water, and then dried to obtain 407.95 g (1.73 mols) of tetrafluoroisophthalamide as a white solid (yield 98.8%).

出典