2-CHLOROPYRIMIDINE-4-CARBOXAMIDE synthesis
- Product Name:2-CHLOROPYRIMIDINE-4-CARBOXAMIDE
- CAS Number:22536-66-9
- Molecular formula:C5H4ClN3O
- Molecular Weight:157.56
149849-92-3
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22536-66-9
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$30.00/100mg
Yield:22536-66-9 92%
Reaction Conditions:
Stage #1: 2‐chloropyrimidine‐4‐carboxylic acidwith thionyl chloride in toluene; for 10 h;Reflux;
Stage #2: with ammonium hydroxide at 20; for 1 h;Cooling with ice;
Steps:
3 Example 3
A 100 mL three-necked reaction flask was added with 50 mL of thionyl chloride, and 2-chloro-pyrimidine-4-carboxylic acid (2c) (15.9 g, 100 mmol) was added in batches under stirring conditions, and the addition was completed in 10 minutes. After the addition, the reaction mixture was refluxed and reacted for 10 hours, the thionyl chloride was distilled off, and 10 mL of N,N-dimethylformamide was added to the residue to dissolve. In addition, 150 mL of ammonia water (25-28% content) was added to a 250 mL three-necked reaction flask, cooled in an ice water bath, and the above acid chloride solution was dripped at constant pressure, and reacted at room temperature for 1 hour after dripping. After the reaction, it was filtered, the solid was washed with 3×20 mL of water, and dried to obtain the solid product 2-chloro-pyrimidine-4-carboxamide (3c) (14.5 g, yield 92%). The target product was confirmed by nuclear magnetic resonance spectroscopy.
References:
CN112851677,2021,A Location in patent:Paragraph 0030-0033
75833-38-4
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22536-66-9
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$30.00/100mg
7460-56-2
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22536-66-9
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15231-48-8
106 suppliers
$24.00/250mg
22536-66-9
91 suppliers
$30.00/100mg