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31860-05-6

5-methoxybenzo[d][1,2,3]thiadiazole synthesis

1synthesis methods
-

Yield:31860-05-6 22%

Reaction Conditions:

with hydrogenchloride;sodium nitrite in water at 20; for 0.5 h;

Steps:

17.2 Step 2: Example 17c

To a mixture of Example 17b (11.2 g, 0.062 mol) in water (20 mL) was added aqueous 0.2 N hydrochloric acid (850 mL, 0.13 mol) slowly at rt., sodium nitrite (6.5 g, 0.094 mol) was then added slowly at r.t., the reaction was stirred at r.t. for 30 min. The residue was extracted with EtOAc (200 mL * 2). The combined organic phase was washed with brine, dried over Na2S04, filtrated and concentrated under reduced pressure to give the crude product which was further purified by silica gel chromatography to give the pure product (Example 17c, 2.4 g, yield 22%) as colorless solid.

References:

WO2017/218960,2017,A1 Location in patent:Paragraph 00448