Methyl iodide → 3,5-Difluoro-2-methoxybenzaldehyde

反応式

[F:1][C:2]1[C:3]([OH:11])=[C:4]([CH:7]=[C:8]([F:10])[CH:9]=1)[CH:5]=[O:6].[C:12](=O)([O-])[O-].[K+].[K+].CI>C(#N)C>[F:1][C:2]1[C:3]([O:11][CH3:12])=[C:4]([CH:7]=[C:8]([F:10])[CH:9]=1)[CH:5]=[O:6]

参加物

実験手順

3,5-Difluoro-2-hydroxybenzaldehyde in the form of a crude product (corresponding to 0.35 mol) was dissolved in 800 ml of acetonitrile. 110 g (0.8 mol) of potassium carbonate and 61 ml (0.96 mol) of methyl iodide were added thereto, and the mixture was heated under reflux for 5 hr. After cooling the mixture, insolubles were removed by filtration, and the mother liquor was concentrated. 1.3 l of ether was added to the concentrate, and the mixture was washed twice with 500 ml of water. Then, the mixture was washed with a saturated saline solution, and the ether layer was dried over anhydrous magnesium sulfate. The solvent was distilled off in vacuo to prepare 39.6 g (yield: 66%) of the intended product (in two states).