1(6H)-Pyridazineacetic acid, 3-methyl-6-oxo-, ethyl ester synthesis
- Product Name:1(6H)-Pyridazineacetic acid, 3-methyl-6-oxo-, ethyl ester
- CAS Number:874491-31-3
- Molecular formula:C9H12N2O3
- Molecular Weight:196.2
Yield:874491-31-3 99.9%
Reaction Conditions:
with potassium carbonate in acetonitrile;Reflux;
Steps:
6.1.9. General procedures for 9a-j and 13a,b
General procedure: A mixture of the suitable intermediate 8a-j, 7 [16] or 12 [31,39] (4.50 mmol), K2CO3 (9.00 mmol), and ethyl bromoacetate (6.75 mmol) in CH3CN (10 mL) was refluxed while stirring for 2-4 h. The mixture was then concentrated in vacuo, diluted with cold water, and extracted with CH2Cl2 (3×15 mL). The solvent was evaporated in vacuo, and compounds 9a-j and 13a,b were purified by crystallization from ethanol (compounds 9b-d,g) or by flash column chromatography using cyclohexane/ethyl acetate 1:1 (for 9a,e,f and 13a,b) and cyclohexane/ethyl acetate 2:1 (for 9h-j) as eluents.
References:
Giovannoni, Maria Paola;Schepetkin, Igor A.;Cilibrizzi, Agostino;Crocetti, Letizia;Khlebnikov, Andrei I.;Dahlgren, Claes;Graziano, Alessia;Dal Piaz, Vittorio;Kirpotina, Liliya N.;Zerbinati, Serena;Vergelli, Claudia;Quinn, Mark T. [European Journal of Medicinal Chemistry,2013,vol. 64,p. 512 - 528] Location in patent:supporting information
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