2,3-Difluoro-4-iodopyridine → 3-Fluoro-4-iodopyridin-2(1H)-one
反応式
F[C:2]1[C:7]([F:8])=[C:6]([I:9])[CH:5]=[CH:4][N:3]=1.C(O)(=[O:12])C.O>>[F:8][C:7]1[C:2](=[O:12])[NH:3][CH:4]=[CH:5][C:6]=1[I:9]参加物
3
実験手順
2,3-Difluoro-4-iodopyridine (300 mg, 1.24 mmol) was suspended in acetic acid:water (2:1, 15 mL). The mixture was heated to reflux and stirred at this temperature overnight. Reaction was concentrated to dryness, and triturated in water (10 mL) for 30 min. The solid was collected via filtration, washed with water (2×10 mL), and pentane (2×20 mL) and dried under vacuum to afford the title compound as a white solid (354 mg, 71.4%). LC-MS m/z 342.0 (M+1). 1H NMR (400 MHz, METHANOL-d4) δ ppm 6.56-6.82 (m, 1 H) 6.83-7.18 (m, 1 H).
後処理
- temperatureThe mixture was heated
- temperatureto reflux
- customReaction
- concentrationwas concentrated to dryness
- customtriturated in water (10 mL) for 30 min
- filtrationThe solid was collected via filtration
- washwashed with water (2×10 mL), and pentane (2×20 mL)
- customdried under vacuum
出典と根拠
- ORDレコード
- ord-a31732891a644086a6103ec424cb8cda
- 出典データセット
- uspto-grants-2014_09
- 特許番号
- US08846933B2
反応ノート
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