Synthesis method of 2-amino-5-chlorobenzophenone
A technology of chlorobenzophenone and synthesis method, which is applied in chemical instruments and methods, preparation of organic compounds, organic chemistry, etc., can solve the problems of expensive phenylboronic acid, harsh absolute anhydrous conditions, environmental pollution, etc., and achieve the reaction time Short, waste reduction, high yield effect
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Embodiment 1
[0019] The synthetic method of 2-amino-5-chlorobenzophenone comprises the following steps:
[0020] (1) Mix ethanol, sodium hydroxide, p-chloronitrobenzene, and phenylacetonitrile with a mass concentration of 95%, first stir at 2000rpm for 30min, and then ultrasonically oscillate at 25°C for 1h. The conditions for ultrasonic oscillation are: Ultrasonic power 100W, frequency 40Hz; Among them, the mass ratio of ethanol, sodium hydroxide, p-chloronitrobenzene, and phenylacetonitrile with a mass concentration of 95% is 10:1.2:2:1.7;
[0021] (2) Microwave the product of step (1) under the condition of 200W power for 10min, add water to the system, filter, wash the filter residue with methanol for 3 times, and then dry it at 80°C for 5h to obtain 5- Chloro-3-phenyl-2,1-benzisoxazole;
[0022] (3) Mix tetrahydrofuran and triethylamine, then add 5-chloro 3-phenyl-2,1-benzisoxazole and palladium carbon catalyst to mix, pass nitrogen gas, replace air 8 times, and then pass hydrogen ga...
Embodiment 2
[0024] The synthetic method of 2-amino-5-chlorobenzophenone comprises the following steps:
[0025] (1) Mix ethanol, sodium hydroxide, p-chloronitrobenzene, and phenylacetonitrile with a mass concentration of 95%, first stir at 2000rpm for 30min, and then ultrasonically oscillate at 35°C for 1h. The conditions for ultrasonic oscillation are: Ultrasonic power 200W, frequency 40Hz; Among them, the mass ratio of ethanol, sodium hydroxide, p-chloronitrobenzene, and phenylacetonitrile with a mass concentration of 95% is 10:1.2:2:1.7;
[0026] (2) Heat the product of step (1) in a microwave for 10 minutes under the condition of a power of 400W, add water to the system, filter, wash the filter residue with methanol for 3 times, and then dry it at 80°C for 5 hours to obtain 5- Chloro-3-phenyl-2,1-benzisoxazole;
[0027] (3) Mix tetrahydrofuran and triethylamine, then add 5-chloro-3-phenyl-2,1-benzisoxazole and palladium-carbon catalyst to mix, pass in nitrogen, replace the air 10 tim...
Embodiment 3
[0029] The synthetic method of 2-amino-5-chlorobenzophenone comprises the following steps:
[0030] (1) Mix ethanol, sodium hydroxide, p-chloronitrobenzene, and phenylacetonitrile with a mass concentration of 95%, first stir at 2000rpm for 30min, and then ultrasonically oscillate at 30°C for 1h. The conditions for ultrasonic oscillation are: Ultrasonic power 200W, frequency 40Hz; Among them, the mass ratio of ethanol, sodium hydroxide, p-chloronitrobenzene, and phenylacetonitrile with a mass concentration of 95% is 10:1.2:2:1.7;
[0031] (2) Microwave the product of step (1) for 10 minutes under the condition of a power of 300W, add water to the system, filter, wash the filter residue with methanol for 3 times, and then dry it at 80°C for 5 hours to obtain 5- Chloro-3-phenyl-2,1-benzisoxazole;
[0032] (3) Mix tetrahydrofuran and triethylamine, then add 5-chloro 3-phenyl-2,1-benzisoxazole and palladium carbon catalyst to mix, pass nitrogen gas, replace air 9 times, and then p...
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