Synthesis method of high-purity bacteriostatic agent and derivatives thereof
A synthesis method and technology of derivatives, applied in the direction of organic chemistry, etc., can solve the problems of difficulty in obtaining high-purity monofluorinated derivatives of fenzazam and the inability to obtain difluoro and trifluoro derivatives, so as to avoid purification loss and cost Low, increased stability effect
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Embodiment 1
[0038] A kind of synthetic method of high-purity bacteriocin and its derivatives of the present invention comprises the following specific steps:
[0039] S1, perchloromethanethiol and primary amine or secondary amine react to prepare intermediate 1 shown in chemical formula 1,
[0040] Wherein R1 and R2 represent aryl, alkyl, alkoxy or their corresponding derivatives, the specific steps are: add primary amine or secondary amine to the solvent, then add perchloromethanethiol, and react at room temperature for 14-18 Hours, the reaction solution was washed with water, separated, dried and concentrated to obtain the intermediate 1;
[0041] S2, the above intermediate 1 is fluorinated with metal or non-metallic fluoride to prepare intermediate 2 shown in chemical formula 1
[0042] Where R1 and R2 represent aryl, alkyl, alkoxy or their corresponding derivatives, X represents fluorine or chlorine, MF nRepresents metal or non-metal fluoride, the specific steps are: mix interme...
Embodiment 2
[0048] Based on Example 1, this example screened the reaction conditions in step S1, the specific steps are as follows:
[0049] (1) With dichloromethane as solvent, isopropylamine and perchloromethanethiol are reaction raw materials
[0050]
[0051] The specific steps are: in a 250mL three-necked flask, add 12.4g of isopropylamine and 94.5mL of dichloromethane in sequence, under the protection of nitrogen, cool down in an ice bath to 0-10°C, and dropwise add 18.6g of perchloromethanethiol, dropwise There was a noticeable heat release during the process. After the dropwise addition was completed, the ice bath was removed, and the temperature was naturally raised to 20-25°C to react overnight. During the reaction, a large amount of white solids gradually precipitated. The reaction solution was washed three times with 50 mL of deionized water, separated, and the organic phase was collected. The organic phase was dried with anhydrous sodium sulfate, filtered, concentrated un...
Embodiment 3
[0078] Based on the above-mentioned embodiments, the present embodiment screens the reaction conditions in step S2, and the specific steps are as follows:
[0079] (1) In a 250mL three-necked flask, add 22.3g of N-[(trichloromethyl)sulfur]diethylamine, 111.5mL of toluene and 11.3g of ferric trifluoride in sequence, and heat up to 105-108°C to react overnight. After the reaction was completed, cool to room temperature, filter, and concentrate the filtrate under reduced pressure to distill off the solvent to obtain 20.1 g of the crude product. Distill under reduced pressure at P=2-4 mmHg, collect fractions at T=52-55°C, and obtain 10.9 g of light yellow liquid, intermediate 2 yield 53%, GC purity 99.0%, the reaction is as follows:
[0080]
[0081] (2) In a 250 mL three-necked flask, add 22.0 g of N-[(trichloromethyl)sulfur]pyrrole, 110.0 mL of toluene and 11.3 g of ferric trifluoride in sequence, and raise the temperature to 105-108° C. to react overnight. After the reactio...
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