A kind of preparation method of multi-substituted fluorine-containing bromophenol benzoic acid
A technology of bromophenol benzoic acid and multi-substitution, which is applied in the field of preparation of multi-substituted fluorine-containing bromophenol benzoic acid, can solve the problems of inconvenient vibration operation of an extraction device, difficult implementation of an extraction link, small volume of an extraction device, and the like, and achieves good preparation effect, solving the problem of demulsification, and the effect of sufficient fixing strength
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Embodiment 1
[0054] An ultrasonic extraction device is characterized in that it comprises an extraction part 1 , a shell part 2 , an ultrasonic part 3 , a crossbar part 4 , a left support part 5 , a right support part 6 , a glass vessel 7 , and a demulsification component 8 . The extraction device can be divided into multiple specifications, for example, the volume of the extraction part can be 1L, 2L, 3L, 4L, 5L to meet different needs.
[0055] The extraction part 1 includes a cylindrical part 11 , an upper opening 12 , an upper cover 13 , a cone part 14 , a liquid stopper group 15 , and a liquid outlet 16 . The main part of the extraction part 1 is formed by splicing an upper opening 12, a cylindrical part 11 and a cone part 14 from top to bottom. 121, the outer edge of the upper cover 13 and the frosted part 121 is a frosted surface, the upper center of the upper cover 13 has a handle part 131, the cone part 14 is in a hollow cone shape, and there is a hole between the cone part 14 and...
Embodiment 2
[0064] A method for preparing a polysubstituted fluorine-containing bromophenol benzoic acid, because it requires a large amount of extraction, is carried out by using an ultrasonic extraction device as described above, and is characterized in that it comprises the following steps.
[0065] (1) Add 3L of water in a larger four-necked bottle, under vigorous stirring, slowly add 740-760g of anhydrous sodium sulfate, 172-180g of hydroxylamine hydrochloride and 190-198g of chloral hydrate successively, keeping the system temperature at about 40 Celsius, 100g of 2,3-difluoroaniline and 200ml of hydrochloric acid were dissolved in 500ml of water to form a mixture, and added to it at one time. After the addition was completed, a condensing device was set up, and the temperature was raised to reflux, and the reaction was continued for 15 minutes. After TLC After confirming that the reaction was completed, the temperature was lowered to 0°C with an external ice-water mixture, a solid wa...
Embodiment 3
[0073] A preparation method of polysubstituted fluorine-containing bromophenol benzoic acid, because it requires a large amount of extraction, uses an ultrasonic extraction device as described above to carry out, and is characterized in that, it comprises the following steps.
[0074] (1) add 3L of water in a larger four-necked flask, under vigorous stirring, slowly add 740g of anhydrous sodium sulfate, 171g of hydroxylamine hydrochloride and 190g of chloral hydrate successively, keep the system temperature at about 40 degrees Celsius, add 98g of 2 , 3-Difluoroaniline and 196ml of hydrochloric acid were dissolved in 500ml of water to form a mixture, and added to it at one time. After the addition was completed, a condenser was set up, and the temperature was raised to reflux, and the reaction was continued for 15 minutes. After confirming that the reaction was completed by TLC, use The external ice-water mixture was cooled to 0 degrees, a solid was precipitated, suction filtere...
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Abstract
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