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113302-88-8

1H-Indazole, 5-Methyl-7-nitro- synthesis

6synthesis methods
-

Yield:113302-88-8 36.6%

Reaction Conditions:

with acetic acid;sodium nitrite in water at 20; for 2 h;

Steps:

24.1 Step 1: Example 24b

To a solution of Example 24a (10.0 g, 60.24 mmol, 1.0 eq) in AcOH (150 mL) was added a solution of NaNO2 (4.99 g, 72.29 mmol, 1.2 eq) in H2O (10 mL) dropwise at r.t. The reaction mixture was stirred for 2 h at r.t. Then, water (100 mL) was added to the mixture, which was stirred for 30 min. The precipitated solid was collected by filtration, which was washed with H2O and MTBE. The crude product was purified by silica gel flash column chromatography to afford the desired product Example 24b (3.9 g, 36.6% yield) as a yellow solid. LCMS [M+1]+ = 178.2.

References:

WO2020/185755,2020,A1 Location in patent:Paragraph 00410

66620-31-3 Synthesis
Benzaldehyde, 2-hydroxy-5-methyl-3-nitro-

66620-31-3
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1H-Indazole, 5-Methyl-7-nitro-

113302-88-8
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