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ChemicalBook CAS DataBase List 2-Chlorobenzothiazole

2-Chlorobenzothiazole synthesis

12synthesis methods
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Yield:615-20-3 95.3%

Reaction Conditions:

with chlorine;trichlorophosphate in chlorobenzene at 80 - 100;Reagent/catalyst;Temperature;Solvent;

Steps:

1-5 Example 4:

With a cooler and a hydrogen chloride tail gas absorption device,Can be stirred and equipped with a chlorine gas introduction tubeIn a 2000 ml reaction flask,600 g of benzothiazole, 500 g of chlorobenzene and 10 g of phosphorus oxychloride catalyst were introduced, and the temperature was raised to 80 ° C.Start to pass chlorine gas at (3 ~ 5) g / min, the reaction is maintained at (80 ~ 100) ° C. Insulation reaction until the HPLC detection of the benzothiazole content in the system is less than 0.5%, the chlorine is stopped, the amount of chlorine is about 300 grams . After the reaction, the nitrogen gas is purged of excess chlorine, which is a 2-chlorobenzothiazole chlorobenzene solution.After distillation under reduced pressure, chlorobenzene and a small amount of raw materials are removed for the next batch.The remaining material was subjected to a high vacuum of 0.099 mPa, and distilled to 165 ° C to obtain 2-chlorobenzothiazole, 725 g, content 99%.The yield was 95.3%.

References:

CN109456282,2019,A Location in patent:Paragraph 0017-0024

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