3,5-PYRAZOLEDICARBOXYLIC ACID synthesis
- Product Name:3,5-PYRAZOLEDICARBOXYLIC ACID
- CAS Number:3112-31-0
- Molecular formula:C5H4N2O4
- Molecular Weight:156.1
67-51-6
518 suppliers
$6.00/25g
3112-31-0
210 suppliers
$18.00/1g
402-61-9
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$10.00/500mg
Yield:3112-31-0 33% ，402-61-9 18%
Reaction Conditions:
with potassium permanganate in water at 70 - 90;
Steps:
1H-Pyrazole-3,5-dicarboxylic acid (1).
3,5-Dimethyl-1H-pyrazole, 78.5 g (0.818 mol), was dissolved in 700 mL of water heated to 70°C, and 517 g (3.271 mol) of potassium permanganate was added to the hot solution, maintaining the temperature no higher than 90°C. The mixture was cooled to room temperature, the precipitate of MnO2 was filtered off and washed with water, and the filtrate was acidified with aqueous HCl to pH 2 and left overnight. The precipitate was filtered off and washed with water. Yield 41.75 g (33%), white crystals, mp 257-258°C. 1H NMR spectrum: δ 7.07 ppm, s (1H, 4-H). 5-Methyl-1H-pyrazole-3-carboxylic acid (2). The aqueous filtrate obtained after separation of diacid 1, was neutralized to pH 5-6, and the precipitate of 2 was filtered off and washed with water. Yield 18.1 g (18%), white crystals, mp 210-211°C. 1H NMR spectrum, δ, ppm: 2.25 s (3H, CH3), 6.42 s (1H, 4-H).
References:
Kharaneko [Russian Journal of Organic Chemistry,2016,vol. 52,# 9,p. 1322 - 1325][Zh. Org. Khim.,2016,vol. 52,# 9,p. 1334 - 1337,4]
67-51-6
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$6.00/25g
3112-31-0
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$18.00/1g
148832-75-1
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3112-31-0
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14090-87-0
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3112-31-0
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$18.00/1g
37687-24-4
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3112-31-0
210 suppliers
$18.00/1g