Production of tolyl-triazone
A technology of toltriazinone and a new method is applied in the new field of preparation of toltriazinone, and can solve the problems of large injury to production and operation workers, strong phosgene toxicity, inability to purify and the like
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[0026] ① Synthesis of 3-methyl-4-(4-trifluoromethylthio)phenoxybenzene isocyanate (2):
[0027] Dissolve 299g of 3-methyl-4-(4-trifluoromethylthio)phenoxyaniline (1) in 5000ml of anhydrous toluene, feed hydrogen chloride to saturation, and add 200g of hexachlorohydrin dropwise under zero-degree cooling Add the solution of dimethyl carbonate / 2000ml toluene in about 4 hours, then slowly raise the temperature to reflux and keep it warm for 4 hours, remove the toluene under reduced pressure, and distill to receive 160℃~166℃ / 1mmHg fraction to obtain 3- Methyl-4-(4-trifluoromethylthio)phenoxybenzene isocyanate (2) 305g, yield 93%;
[0028] ② 1(N)-acetyl-2(N)-methyl-3(N)-[3-methyl-4-(4-trifluoromethylthio)phenoxy]phenyltriurea (3) preparation:
[0029] Dissolve 162.5 g of 3-methyl-4-(4-trifluoromethylthio)phenoxybenzene isocyanate (2) in 500 ml of chloroform, add 70 g of N-acetyl-N'-methylurea, Heating and reflux reaction, followed by TLC until the disappearance of the raw materia...
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