Acetyl chloride → Ethyl 3-(3,4-difluorophenyl)propanoate
反応式
[F:1][C:2]1[CH:3]=[C:4]([CH2:9][CH2:10][C:11]([OH:13])=[O:12])[CH:5]=[CH:6][C:7]=1[F:8].[C:14](Cl)(=O)[CH3:15]>CCO>[F:1][C:2]1[CH:3]=[C:4]([CH2:9][CH2:10][C:11]([O:13][CH2:14][CH3:15])=[O:12])[CH:5]=[CH:6][C:7]=1[F:8]参加物
4
実験手順
To a solution of 3-(3,4-difluorophenyl)propionic acid (1.0 g, 5.4 mmol) in EtOH (10 mL) is added dropwise acetyl chloride (1.0 mL, 14.1 mmol), and the solution is stirred at RT for 2 h. The solvent is rotary evaporated, and the residue purified by chromatography on silica gel; elution with heptane:EtOAc (4:1) gives 0.99 g of the product 249. 1H NMR (CDCl3) δ 7.10-6.85 (m, 3 H), 4.13 (q, 2 H), 2.90 (t, 2 H), 3.35-2.59 (t, 2 H), 1.23 (t, 2 H); MS: m/z 215 (M++1).
後処理
- customthe residue purified by chromatography on silica gel
- washelution with heptane:EtOAc (4:1)
出典と根拠
- ORDレコード
- ord-40824b40e7724892b98cde21d9fdf733
- 出典データセット
- uspto-grants-2010_06
- 特許番号
- US07741493B2
反応ノート
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