Hydrochloric Acid → Ethanone, 1-[2-methoxy-4-(methylthio)phenyl]-
反応式
[CH3:1][S-:2].[Na+].F[C:5]1[CH:10]=[CH:9][C:8]([C:11](=[O:13])[CH3:12])=[C:7]([O:14][CH3:15])[CH:6]=1.Cl>CN(C=O)C>[CH3:15][O:14][C:7]1[CH:6]=[C:5]([S:2][CH3:1])[CH:10]=[CH:9][C:8]=1[C:11](=[O:13])[CH3:12]参加物
5
実験手順
Sodium thiomethoxide (1.3 g, 18.5 mmol) in DMF (15 ml) was added to 1-(4-fluoro-2-methoxyphenyl)ethanone (2.85 g, 16.9 mmol) in DMF (5 ml). The mixture was stirred for overnight at room temperature. HCl (1%) was added, the water phase was extracted with EtOAc, the combined organic phases were washed with LiCl (5%), brine and were concentrated to give the title compound (3.6 g) MS m/z (rel. intensity, 70 eV) 196 (M+, 35), 182 (11), 181 (bp), 166 (8), 136 (10).
後処理
- extractionthe water phase was extracted with EtOAc
- washthe combined organic phases were washed with LiCl (5%), brine
- concentrationwere concentrated
出典と根拠
- ORDレコード
- ord-3ef35471bd594085b123d7f59d663396
- 出典データセット
- uspto-grants-2013_09
- 特許番号
- US08524766B2
反応ノート
読み込み中…