反応式
[C:1]([O:4][C:5]1[CH:10]=[CH:9][C:8]([O:11]C=O)=[CH:7][C:6]=1[O:14]C)(=O)C.O.[Li+].[OH-]>C1COCC1>[CH3:1][O:4][C:5]1[CH:10]=[CH:9][C:8]([OH:11])=[CH:7][C:6]=1[OH:14]参加物
5
実験手順
To a solution of 4-(formyloxy)-2-methoxyphenyl acetate (16 g, 76 mmol) in THF (50 mL)/H2O (50 mL) was added LiOH (7.7 g, 184.2 mmol). The reaction was stirred at room temperature overnight. The volatiles were removed under reduced pressure. The residue was extracted with EA (50 mL×3). The organic phase was washed with brine (50 mL), dried over Na2SO4, filtrated and concentrated in vacuo to give black oil, which was purified by silica gel column (PE:EA=3:1) to afford 4.8 g of product (40%) as a brown solid.
後処理
- customThe volatiles were removed under reduced pressure
- extractionThe residue was extracted with EA (50 mL×3)
- washThe organic phase was washed with brine (50 mL)
- dry with materialdried over Na2SO4
- filtrationfiltrated
- concentrationconcentrated in vacuo
- customto give black oil, which
- customwas purified by silica gel column (PE:EA=3:1)
出典と根拠
- ORDレコード
- ord-3677ef16c4504ba28f17d096acf43e67
- 出典データセット
- uspto-grants-2013_07
- 特許番号
- US08481590B2
関連ノート
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