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ChemicalBook CAS DataBase List Benzothiazole, 5,6-dimethoxy- (9CI)

Benzothiazole, 5,6-dimethoxy- (9CI) synthesis

2synthesis methods
-

Yield:58249-69-7 86%

Reaction Conditions:

with potassium sulfide;ammonium acetate in water at 140; for 12 h;Schlenk technique;Inert atmosphere;

Steps:

2

In the dry Schlenk reaction tube, add 3,4-dimethoxyaniline (0.3mmol),Potassium sulfide (0.9mmol), dimethyl sulfoxide (2ml), ammonium acetate (1.2mmol) and water (80 uL), after the sample is added, use an oil pump to vacuum and inject nitrogen for gas replacement, after three replacements, the reaction is stopped at 140°C for 12 hours and then cooled to room temperature. The reaction is detected by thin layer chromatography (TLC), after the reaction of the raw materials is completed, the reaction is terminated, and the mixture in the reaction tube is cooled to room temperature. Preliminary treatment of the mixed solution: extraction, collecting the organic layer, spinning powder, and performing column chromatography to obtain the target product with a yield of 86%.

References:

CN111793042,2020,A Location in patent:Paragraph 0027-0029