5-AMINO-1-(3-CHLOROPHENYL)-1H-PYRAZOLE-& synthesis
- Product Name:5-AMINO-1-(3-CHLOROPHENYL)-1H-PYRAZOLE-&
- CAS Number:51516-68-8
- Molecular formula:C10H7ClN4
- Molecular Weight:218.64
2312-23-4
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123-06-8
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51516-68-8
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Yield:51516-68-8 72%
Reaction Conditions:
with potassium etoxide;sodium hydride in ethanol at 0; for 1 h;Heating / reflux;
Steps:
1.1a.1.2A
Sodium hydride as a 60% dispersion in mineral oil (0.48 g, 1.2 eq, 12 mmol) was added slowly to ethanol (20 ml) at 0°C. To the solution of sodium ethoxide in ethanol was added 3-chlorophenylhydrazine hydrochloride (1.79 g, 1.0 eq, 10 mmol), addition of ethoxymethylene malonitrile (1.22 g, 1.0 eq, 10 mmol) shortly followed. The reaction mixture was heated to reflux with stirring for 1 hour. The reaction mixture was then allowed to cool to room temperature, once at room temperature a precipitate was observed. Ethanol (20 ml) was added to the slurry and the precipitate was collected by filtration, washed with diethyl ether (2 x 100 ml) and dried in vacuo to give the title compound as a yellow solid (1.56 g, 7.13 mmol, 72%). LCMS: [M+H]+=219, Rt = 1.17 min, 100% purity.
References:
EP1746099,2007,A1 Location in patent:Page/Page column 14
123-06-8
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14763-20-3
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51516-68-8
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108-42-9
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51516-68-8
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122-51-0
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14763-20-3
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109-77-3
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51516-68-8
56 suppliers
$12.00/250mg