1-(4-FLUOROPHENYL)-3-METHYL-1H-PYRAZOLE-5-CARBOXYLIC ACID ETHYL ESTER synthesis
- Product Name:1-(4-FLUOROPHENYL)-3-METHYL-1H-PYRAZOLE-5-CARBOXYLIC ACID ETHYL ESTER
- CAS Number:288251-64-9
- Molecular formula:C13H13FN2O2
- Molecular Weight:248.25
823-85-8
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Yield:-
Reaction Conditions:
with potassium acetate in ethanol;
Steps:
1.A
4-Fluorophenylhydrazine hydrochloride (25.0 g, 0.154 mol) was added in one portion to a solution of potassium acetate (16.6 g, 0.169 mol) and ethyl acetopyruvate (24.3 g, 0.154 mol) in ethanol (0.154 L). After stirring overnight, methyl tert-butyl ether (0.150 L) was added, the resulting solid was removed by filtration, and the filtrate was concentrated to 40 g of dark oil. This was dissolved in chloroform (100 g), divided into two equal portions, and each portion was purified by prep ηPLC (silica cartridge, eluting with 25% to 40% ethyl acetate in hexane) to separate the two pyrazole isomers. The fractions from both purifications that contained the lower running isomer were combined and concentrated to yield 15.81 g of ethyl l-(4-fluorophenyl)-5-methyl-lH-pyrazole-3- carboxylate as an orange oil. The fractions from both purifications that contained the higher running isomer were combined and concentrated to yield 9.58 g of ethyl l-(4- fluoroρhenyl)-3-methyl-lH-pyrazole-5-carboxylate as an orange solid.
References:
WO2007/79086,2007,A1 Location in patent:Page/Page column 83
371-14-2
88 suppliers
inquiry
615-79-2
258 suppliers
$8.00/5g
126129-41-7
0 suppliers
inquiry
288251-64-9
25 suppliers
$165.00/1g