5-Bromo-4-chlorothiophene-2-sulfonamide → 4-Chlorothiophene-2-sulfonamide
反応式
Br[C:2]1[S:6][C:5]([S:7]([NH2:10])(=[O:9])=[O:8])=[CH:4][C:3]=1[Cl:11]>CC(O)=O.[Zn]>[Cl:11][C:3]1[CH:4]=[C:5]([S:7]([NH2:10])(=[O:9])=[O:8])[S:6][CH:2]=1参加物
4
反応条件
- 温度
- 120 °C
実験手順
To a stirred solution of 5-bromo-4-chlorothiophene-2-sulfonamide (2.4 g, 8.7 mmol) in AcOH (20 mL) is added zinc dust (1.7 g, 26.0 mmol). The reaction mixture is heated to 120° C. for 6 hr. After 6 hr, the mixture is filtered and neutralized with 1 M NaOH. The aqueous layer is extracted with EtOAc (2×100 mL). The combined organic extracts are dried (Na2SO4), filtered and concentrated in vacuo. The crude product is chromatographed on silica gel, eluting with CH2Cl2 to afford the title compound (0.88 g, 52%).
後処理
- filtrationthe mixture is filtered
- extractionThe aqueous layer is extracted with EtOAc (2×100 mL)
- dry with materialThe combined organic extracts are dried (Na2SO4)
- filtrationfiltered
- concentrationconcentrated in vacuo
- customThe crude product is chromatographed on silica gel
- washeluting with CH2Cl2
出典と根拠
- ORDレコード
- ord-ee96dca7353343b0ab451e1a1c0600f7
- 出典データセット
- uspto-grants-2006_08
- 特許番号
- US07084170B2
反応ノート
読み込み中…