3-Methylpyridazine 2-oxide synthesis
- Product Name:3-Methylpyridazine 2-oxide
- CAS Number:19602-00-7
- Molecular formula:C5H6N2O
- Molecular Weight:110.11
1632-76-4
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Yield:19602-00-7 41%
Reaction Conditions:
with dihydrogen peroxide;glacial acetic acid in lithium hydroxide monohydrate at 120; for 6 h;
Steps:
Synthesis of 6-methylpyridazine 1-oxide
Synthesis of 6-methylpyridazine 1-oxideTo a solution of 3-methylpyridazine (4.60 g, 48.9 mmol) in acetic acid (30.0 mL) was added H202 (29.4 g,259 mmol, 29.4 mL, 30% (w/w) in water). The mixture was heated at 120 °C for 6 h. The mixture wasallowed to cool to RT and poured in aqueous saturated NaHCO3 (500 mL) and extracted with DCM (5x 50 mL). The combined organic layer was dried over Na2SO4 and concentrated in vacuo to afford 6- methylpyridazine 1-oxide (2.22 g, 20.2 mmol, 41%). LCMS: caic. for [M+H] = 111.05, found 111.2. 1H- NMR shows a 1:1 mixture of both possible N-oxides.
References:
WO2015/161928,2015,A1 Location in patent:Page/Page column 60; 70; 71
