Acetic Anhydride → (3-Methylthiophen-2-yl)methyl acetate
反応式
[CH3:1][C:2]1[CH:6]=[CH:5][S:4][C:3]=1[CH2:7][OH:8].[C:9](OC(=O)C)(=[O:11])[CH3:10]>N1C=CC=CC=1.CCOC(C)=O>[C:9]([O:8][CH2:7][C:3]1[S:4][CH:5]=[CH:6][C:2]=1[CH3:1])(=[O:11])[CH3:10]参加物
5
実験手順
To a solution of 62.2 (0.87 g, 6.79 mmol) in pyridine (20 mL) was added acetic anhydride (0.8 mL, 8.14 mmol) at room temperature. The mixture was stirred overnight at room temperature, diluted with EtOAc, washed with 1N HCl and brine, dried (Na2SO4), and concentrated. The crude product was chromatographed on silica gel (0-15% EtOAc/hexane) to afford 62.3. 1H NMR (400 MHz, CDCl3) δ 7.21 (d, 1H), 6.84 (d, 1H), 5.20 (s, 2H), 2.26 (s, 3H), 2.08 (s, 3H).
後処理
- washwashed with 1N HCl and brine
- dry with materialdried (Na2SO4)
- concentrationconcentrated
- customThe crude product was chromatographed on silica gel (0-15% EtOAc/hexane)
出典と根拠
- ORDレコード
- ord-c083b74b5d2a4ba4ada4e6e999eaae8d
- 出典データセット
- uspto-grants-2010_05
- 特許番号
- US07714008B2
反応ノート
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