반응 #46940

반응 방정식

sulfuric acid

tetrafluoroisopthalonitrile

water

sulfuric acid

→

tetrafluoroisophthalamide

수율 98.9%

반응 조건

후처리

1. 1
   온도kept 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
   기타was kept at 90 to 100° C.
6. 6
   기타from exceeding 60° C
7. 7
   workup.ADDITIONAfter the completion of the dropwise addition
8. 8
   온도the mixture was cooled to 20° C.
9. 9
   기타A white solid which was precipitated
10. 10
    기타was separated by filtration
11. 11
    세척washed with 1000 g of water
12. 12
    기타dried

실험 절차

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%).

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