Fluazinam synthesis
- Product Name:Fluazinam
- CAS Number:79622-59-6
- Molecular formula:C13H4Cl2F6N4O4
- Molecular Weight:465.09
29091-09-6
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79456-26-1
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79622-59-6
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Yield:79622-59-6 98%
Reaction Conditions:
with potassium hydroxide in 2-methyltetrahydrofuran at 20; for 4 h;Concentration;Temperature;Solvent;
Steps:
3 Example 3
A mixture of 1.00 mol of 2-amino-3-chloro-5-trifluoromethylpyridine, 1.05 mol of 2,4-dichloro-3,5-dinitro-trifluorotoluene, 4.0Moles of 85% potassium hydroxide and 300 g of 2-methyltetrahydrofuran (0.5% moisture content) were placed in a 2 L four-necked reaction flask,20 ° C was stirred at room temperature for 4 hours.Take 1 drop of the reaction solution in the sampling tube, add 1 drop of dilute hydrochloric acid to the reaction solution pH <6 acidic, and then use acetonitrile as the solution Dilution of the reaction solution to 2ml, and then take 1ml for HPLC detection and external standard method to determine the reaction solution The content of each component in the product after reaction was shown in Table 1. The detection conditions for HPLC were the same as in Example 1.Then, the water was dissolved to clarify, and the organic phase was allowed to stand and the organic phase was subjected to atmospheric distillation at a distillation temperature of less than 100 ° C Shrink and desolate to no liquid distillation, then add a small amount of water beating, filtration, drying at less than 100 after the preparation of fluoride And the weight of the finished product was 457g, and the purity was 99.8% by HPLC with the same detection conditions. The molar yield was98.0%. The results of the identification were the same as in Example 1.
References:
CN106316937,2017,A Location in patent:Paragraph 0047; 0048; 0049; 0050; 0051; 0052; 0053-0080
59-67-6
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79622-59-6
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3099-50-1
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79622-59-6
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69045-83-6
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79622-59-6
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69045-84-7
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79622-59-6
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$50.00/500mg