Ethanone, 1-(4-methoxy-2-pyridinyl)- (9CI) synthesis
- Product Name:Ethanone, 1-(4-methoxy-2-pyridinyl)- (9CI)
- CAS Number:59576-28-2
- Molecular formula:C8H9NO2
- Molecular Weight:151.16
75-16-1
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36057-44-0
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59576-28-2
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Yield:59576-28-2 73%
Reaction Conditions:
Stage #1: methylmagnesium bromide;2-cyano-4-methoxylpyridine in tetrahydrofuran at -78 - 20; for 5.5 h;
Stage #2: with water in tetrahydrofuran;
Steps:
16
[Referential Example 16]; 1-(4-Methoxy-2-pyridyl)ethanone ; [] In an argon atmosphere, 0.93M methylmagnesium bromide in tetrahydrofuran (13.8 mL) was added dropwise to 4-methoxypyridine-2-carbonitrile (1.56 g) in tetrahydrofuran (31 mL) at -78°C, followed by stirring for 15 minutes. Subsequently, the reaction mixture was stirred at 0°C for 15 minutes, and then at room temperature for 5 hours. Water was added dropwise to the reaction mixture. The resultant mixture was partitioned between water and ethyl acetate. The organic layer was dried over sodium sulfate anhydrate, followed by filtration. The solvent was evaporated under reduced pressure, and the residue was purified by silica gel column chromatography (hexane - ethyl acetate), to thereby give the title compound as a solid substance (1.30 g, 73%) .1H-NMR(400MHz,CDCl3) δ: 2.72(3H,s), 3.91(3H,s), 6.97-6.99(1H,m), 7.57-7.58(1H,m), 8.48-8.50(1H,m). MS(ESI)m/z: 152(M+H)+.
References:
EP1591443,2005,A1 Location in patent:Page/Page column 31-32
36057-44-0
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59576-28-2
53 suppliers
$94.25/1g
1122-96-9
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$22.00/1g
59576-28-2
53 suppliers
$94.25/1g