TH3280B - Tricyclazol synthesis - Google Patents

Abstract

A new and effective one-step method for the preparation of high-yielding, additive-free tricyclazol.

Claims (8)

1. Process for preparing tricyclazol having formula (chemical formula) which is characterized by 2-amino-4-methyl benzothiazole with the formula (chemical formula) reacts with hydrazine or hydrate of this substance in the presence of ethylene glycol and hydrochlorates. It was also present at temperatures from about 100 degrees to about 150 degrees to produce 2-hydracino-4-methylbenzothiazone with the formula (chemical formula), which by cooling the mixture. Below about 100 degrees and the addition of xylene Next, cool the mixture from approximately 10 degrees to approximately 45 degrees and allow to separate the ethylene glycol layer. Adding water Let the mixtures separate. Removing the water layer The addition of an acid-destroying agent is not reversed into the xylene layer, which needs to be slightly more than sufficient. To neutralize this mixture The resulting xylene layer was distilled at a liquid temperature of approximately 100 degrees to approximately 120 degrees to remove the water acytotropes and xylene. Further distillation of the mixture to remove the acytotropes of ethylene glycol and xylene. Until the ethylene glycol is considered to have been completely removed, cool the mixture below about 100 degrees if necessary, add a mole of 2-hydrashino-4-methylbenzothiazole continues at least 5.0 moles of formic acid. At a minimum, a concentration of 80% by weight is added to this mixture and this mixture is maintained at high temperatures until a desirable product is formed. 2. Process according to claim 1 where tricyclazole can be recovered by distillation using formic Too much acid gets out of the mix. Add more xylene if needed to make the slurry run smoothly. Combine this mixture with sufficient water to dissolve inorganic impurities. Cool the mixture And separation of crystalline products 3. The process of claim 1 or 2, which is characterized by the addition of xylene in a volume of approximately 40% to approximately 80% of the volume of ethylene glycol. 4. A process according to claim 3, which is characterized by the addition of xylene in a volume of approximately 60% to approximately 70% of the volume of ethylene glycol. 5. Any process of claim 1 through 4 in which the acid-destroying agent is not converted to carbonate. 6. Process according to one of the foregoing claims in which Formic Acid is approximately 85% by weight. 7. Process according to any of the foregoing claims. For each mole of 2-hydracino-4-methylbenzothiazole, 5.0 formic acid was used. 8. Process according to any of the foregoing claims. For each mole of 2-hydracin-4-methylbenzothiazole, 10.5 mol of formic acid was used.