5-amino-1-(2-hydroxyethyl)pyrazole-4-carboxylic acid synthesis
- Product Name:5-amino-1-(2-hydroxyethyl)pyrazole-4-carboxylic acid
- CAS Number:58046-50-7
- Molecular formula:C6H9N3O3
- Molecular Weight:171.15
109-84-2
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Yield:58046-50-7 86.16%
Reaction Conditions:
Stage #1: 2-hydroxyethylhydrazine;2-(4b-dimethylaminomethylene)-2-cyano ethyl acetate in toluene at 100;
Stage #2: with sodium hydroxide at 100;Temperature;Solvent;
Steps:
1.2; 2.2 Synthesis of N-hydroxyethyl-5-amino-1H-pyrazole-4-carboxylic acid
2-cyano-3-(dimethylamino) ethyl acrylate 354.5g (1.948mol), 920g of toluene, 222.1g (2.922mol) of β-hydroxyethylhydrazine, added to a three-necked flask, reacted at 100°C, followed by TLC. After the reaction was completed, remove the solvent, and add 30% NaOH 362g (2.715mol) ), hydrolyzed at 100°C, followed the reaction by TLC, after the reaction was completed, the temperature was lowered, concentrated hydrochloric acid was added to adjust the pH to below 5, and filtered to obtain 287g (1.678mol) of N-hydroxyethyl-5-amino-1H-pyrazole-4-carboxylic acid, Yield 86.16%
References:
CN113135857,2021,A Location in patent:Paragraph 0023; 0026-0027; 0030; 0033-0034
