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ChemicalBook CAS DataBase List 6-FLUORO-5-NITRO-1H-INDAZOLE

6-FLUORO-5-NITRO-1H-INDAZOLE synthesis

7synthesis methods
-

Yield:633327-51-2 30.3%

Reaction Conditions:

with sodium nitrate;sulfuric acid at 0; for 2.5 h;Large scale;

Steps:

5-6 Example 5. Synthesis of Compound II-3

NaNO3 (5100mg, 60mmol) was placed in a 500mL reaction flask.60 mL of concentrated sulfuric acid, 6-fluoroindazole 1 (8167 mg, 60 mmol) were added dropwise thereto at 0 ° C.It was dissolved in 60 mL of concentrated sulfuric acid and the resulting solution was slowly added dropwise to a concentrated sulfuric acid solution of NaNO3, and the reaction was carried out at 0 ° C for 2.5 hours.The reaction solution was poured into 500 mL of ice-water mixture, and filtered with suction paper.The filtrate was extracted with EA, the organic phase and the solid phase obtained by suction filtration were combined and washed with saturated NaHCO3 and saturated NaCl in this order, dried over Na2SO4 and concentrated.Column chromatography (DCM) gave 2:3300 mg (30.3%) of a light yellow solid.

References:

CN110642874,2020,A Location in patent:Paragraph 0489-0491; 0499-0501