* All experimental methods are cited from the reference, please refer to the original source for details. We do not guarantee the accuracy of the content in the reference.
With trichlorophosphate In N,N-dimethyl-formamide at -15 - 20℃; for 7.5 h;
In a 250 mL three-necked flask, 2,4-difluorobenzamide was added(23.0 g, 146.2 mmol) was dissolved in dry formN, N-dimethylformamide (80 mL), cooled to -15 ° C,Phosphorus oxychloride (112. lg, 730.9 mmol) was slowly added dropwise,Incubation reaction 0.5h, room temperature reaction 7h. Reaction is completed,The reaction solution slowly into the ice that is solid precipitation,And 17.0 g of 2,4-difluorobenzonitrile was taken in a yield of 83.4percent.
Reference：
[1] Patent: CN106854165, 2017, A, . Location in patent: Paragraph 0104; 0105; 0136; 0137
2
[ 85118-02-1 ]
[ 67152-20-9 ]
Reference：
[1] Patent: CN106854165, 2017, A,
3
[ 72482-64-5 ]
[ 85118-02-1 ]
Yield
Reaction Conditions
Operation in experiment
95.5%
at -10 - 20℃; for 1.5 h;
In a 250 mL three-necked flask, add ammonia (150 mL), cool to -10 ° C,Dropping concentrated solution, incubation reaction 0.5h,Room temperature reaction lh. The reaction was completed and the filter was filtered and the filter cake was dried in vacuo2,4-difluorobenzamide, 23.8 g, the yield was 95.5percent
Reference：
[1] Patent: CN106854165, 2017, A, . Location in patent: Paragraph 0102; 0103; 0134; 0135
4
[ 1583-58-0 ]
[ 85118-02-1 ]
Reference：
[1] Bioorganic and Medicinal Chemistry, 2006, vol. 14, # 24, p. 8574 - 8581
[2] Patent: CN106854165, 2017, A,
In a 250 mL three-necked flask, add ammonia (150 mL), cool to -10 C,Dropping concentrated solution, incubation reaction 0.5h,Room temperature reaction lh. The reaction was completed and the filter was filtered and the filter cake was dried in vacuo2,4-difluorobenzamide, 23.8 g, the yield was 95.5%
92%
With ammonia; In water; acetone; at 50℃; for 3h;
To a 2000 ml single-mouth bottle, 310 g (1.76 mol) of <strong>[72482-64-5]2,4-difluorobenzoyl chloride</strong>, 500 ml of acetone, and 690 g of aqueous ammonia (10.56 mol) were reacted at 50 C for 3 hours.The acetone was concentrated under reduced pressure, suction filtered, and the filter cake was dried under reduced pressure to give 2,4-difluorobenzamide to give 255 g (1.62 mol).The yield was 92%.
With trifluoroacetic anhydride; In tetrahydrofuran; at 40℃; for 3h;
To a 3000 ml three-necked flask, 283 g (1.80 mol) of 2,4-difluorobenzamide, 600 g of tetrahydrofuran, and 454 g (2.16 mol) of trifluoroacetic anhydride were added dropwise.The reaction was carried out at 40 C for 4 hours. After the reaction was completed, it was washed twice with 600 ml of water, and 600 ml of saturated food.After washing once, the phases were separated, and the organic layer was dried over anhydrous sodium sulfate, filtered, filtered,That is, 2,4-difluorobenzonitrile gave 235 g (1.69 mol) in a yield of 94% and a purity of 99% or more.
83.4%
With trichlorophosphate; In N,N-dimethyl-formamide; at -15 - 20℃; for 7.5h;
In a 250 mL three-necked flask, 2,4-difluorobenzamide was added(23.0 g, 146.2 mmol) was dissolved in dry formN, N-dimethylformamide (80 mL), cooled to -15 C,Phosphorus oxychloride (112. lg, 730.9 mmol) was slowly added dropwise,Incubation reaction 0.5h, room temperature reaction 7h. Reaction is completed,The reaction solution slowly into the ice that is solid precipitation,And 17.0 g of 2,4-difluorobenzonitrile was taken in a yield of 83.4%.
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