反応式
[CH3:1][O:2][C:3]1[C:12]([CH3:13])=[CH:11][CH:10]=[CH:9][C:4]=1[C:5]([O:7]C)=[O:6].[OH-].[K+]>CO.O>[CH3:1][O:2][C:3]1[C:12]([CH3:13])=[CH:11][CH:10]=[CH:9][C:4]=1[C:5]([OH:7])=[O:6]参加物
5
実験手順
To a solution of 2 (1.19 mol) in a mixture of methanol (2 L) and water (0.5 L), potassium hydroxide pellets (100 gram, 1.5 mol) were added under cooling. The mixture was refluxed overnight and evaporated to dryness. The residue was dissolved in water (0.5 L) and acidified with HCl 6N. The product precipitated and 189 g of product was collected as white crystals. Yield 95%. 1H NMR (500 MHz, CDCl3, 25° C.) δ: 2.234 (s, 3H, CH3), 3.717 (s, 3H, OCH3), 7.062 (t, J=7.5, 1H, ArH), 7.365 (d, J=7.5, 1H, ArH), 7.496 (d, J=7.5, 1H, ArH).
後処理
- additionwere added
- temperatureunder cooling
- temperatureThe mixture was refluxed overnight
- customevaporated to dryness
- dissolutionThe residue was dissolved in water (0.5 L)
- customThe product precipitated
- custom189 g of product was collected as white crystals
出典と根拠
- ORDレコード
- ord-dbaf181f786043bd93d9666b8a8a3bf8
- 出典データセット
- uspto-grants-2002_06
- 特許番号
- US06406297B1
関連ノート
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