2H-Indazole, 6-nitro- synthesis
- Product Name:2H-Indazole, 6-nitro-
- CAS Number:65750-02-9
- Molecular formula:C7H5N3O2
- Molecular Weight:163.13
Yield:65750-02-9 84.9%
Reaction Conditions:
with acetic acid at 20; for 1 h;Inert atmosphere;
Steps:
6.02 Step 02: Synthesis of 6-nitro-2H-indazol (03)
To a stirred solution of tert-butyl nitrite (02) (20.3 g, 197.0 mmol, 1.50 equiv) in acetic acid (100.0 mL, 5.0 vol. equiv) was added drop wise a solution of 2-methyl-5-nitroaniline (20.0 g, 131.0 mmol, 1.0 equiv) in acetic acid (400 mL, 20.0 vol. equiv) at RT. The resulting mixture was stirred for lh at RT. The completion of reaction was monitored by TLC (Mf: 30% EtOAc in n-hexane, Rf; 0.4). The reaction mixture was concentrated under vacuum and residue was dissolved in ethyl acetate (500.0 mL). Then residue were washed with sodium bicarbonate solution (150.0 mL), brine (100.0 mL), dried over Na2S04 and concentrated under vacuum to afford titled compound (03) (18.2 g, 84.9%) as a reddish solid. MR (300 MHz, OMSO-d6) δ 13.80 (s, 1H), 8.46 (s, 1H), 8.33 (s, 1H), 8.01 (s, 1H). MS (ES-): 162.20 (M-l).
References:
WO2018/200981,2018,A1 Location in patent:Paragraph 0209; 0230
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