1-Bromo-3,5-difluorobenzene → 1-Bromo-3-fluoro-5-(methylsulfanyl)benzene
反応式
[Br:1][C:2]1[CH:7]=[C:6](F)[CH:5]=[C:4]([F:9])[CH:3]=1.[CH3:10][S-:11].[Na+]>CN(C)C=O>[Br:1][C:2]1[CH:7]=[C:6]([S:11][CH3:10])[CH:5]=[C:4]([F:9])[CH:3]=1参加物
4
反応条件
- 温度
- 150 °C
実験手順
To a solution of 1-bromo-3,5-difluorobenzene (5.0 g, 25.9 mmol) in dimethylformamide (40 ml) was added sodiumthiomethylate (1.81 g, 25.9 mmol), and the mixture was heated to 150° C. for 10 min. The reaction mixture was brought to ambient temperature, quenched with saturated aqueous ammonium chloride (100 ml) and extracted with ethylacetate (3×100 ml). The combined organic phases was dried and concentrated in vacuo to receive the pure title compound (3.84 g). MS m/z (rel. intensity, 70 eV) 222 (M+, 100), 220 (M+, 100), 189 (49), 187 (50), 126 (75).
後処理
- customwas brought to ambient temperature
- customquenched with saturated aqueous ammonium chloride (100 ml)
- extractionextracted with ethylacetate (3×100 ml)
- customThe combined organic phases was dried
- concentrationconcentrated in vacuo
出典と根拠
- ORDレコード
- ord-ef19c52ec3fb43ea8415c457ee1025ab
- 出典データセット
- uspto-grants-2013_08
- 特許番号
- US08501777B2
反応ノート
読み込み中…