![](/CAS/20200515/GIF/1004455-73-5.gif)
1H-Pyrazole-5-carboxylic acid, 3-(1,1-dimethylethyl)-1-methyl-4-nitro- synthesis
- Product Name:1H-Pyrazole-5-carboxylic acid, 3-(1,1-dimethylethyl)-1-methyl-4-nitro-
- CAS Number:1004455-73-5
- Molecular formula:C9H13N3O4
- Molecular Weight:227.22
![3-(TERT-BUTYL)-1-METHYL-1H-PYRAZOLE-5-CARBOXYLIC ACID](/CAS/GIF/175277-11-9.gif)
175277-11-9
95 suppliers
$21.00/250mg
![1H-Pyrazole-5-carboxylic acid, 3-(1,1-dimethylethyl)-1-methyl-4-nitro-](/CAS/20200515/GIF/1004455-73-5.gif)
1004455-73-5
5 suppliers
inquiry
Yield:1004455-73-5 72%
Reaction Conditions:
with sulfuric acid;sulfur trioxide;nitric acid at 0 - 60; for 4 h;
Steps:
2.E
Oleum (816 mmol) is slowly added to fuming nitric acid (890 mmol) at 00C followed by the addition of 5-ter?-butyl-2-methyl-2H-pyrazole-3-carboxylic acid (148 mmol) in small portions. After addition, the reaction mixture is stirred at 600C for 4h. On completion, the reaction mixture is cooled to room temperature and poured into crushed ice. The aqueous phase is then extracted with ethyl acetate (250 mL x 3). The combined organic phases are washed with water (200 mL x 2) and dried over anhydrous sodium sulfate. The solvent is removed under reduced pressure to afford 5-tert-butyl-2-methyl- 4-nitro-2H-pyrazole-3-carboxylic acid as light yellow solid (24.2g, 72%). [0213] 1H NMR (400 MHz, DMSO-^6) δ: 3.96 (s, 3H), 1.29 (s, 9H). Mass (m/z): 228 (M+H).
References:
WO2009/71706,2009,A1 Location in patent:Page/Page column 43-44