반응식
[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]참가 물질
5
실험 절차
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).
후처리
- 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
출처 및 근거
- ORD 기록
- ord-dbaf181f786043bd93d9666b8a8a3bf8
- 출처 데이터셋
- uspto-grants-2002_06
- 특허 번호
- US06406297B1
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