Iodine → HCID 178474489、化合物
反応式
[F:1][C:2]1[CH:3]=[C:4]([C:8]2[CH:12]=[C:11]([NH:13][C:14](=[O:16])[CH3:15])[NH:10][N:9]=2)[CH:5]=[CH:6][CH:7]=1.[I:17](O)(=O)=O.II>C(O)C>[F:1][C:2]1[CH:3]=[C:4]([C:8]2[C:12]([I:17])=[C:11]([NH:13][C:14](=[O:16])[CH3:15])[NH:10][N:9]=2)[CH:5]=[CH:6][CH:7]=1参加物
5
反応条件
- 温度
- 60 °C
実験手順
A suspension of N-[3-(3-fluorophenyl)-1H-pyrazol-5-yl]acetamide (7.6 g, 34.7 mmol), iodic acid (1.5 g, 8.5 mmol) and iodine (4.4 g, 17.3 mmol) in ethanol (200 mL) was heated at 60° C. for 1 h and cooled to room temperature. The reaction mixture was concentrated in vacuo and partitioned between CH2Cl2 and 2 M Na2S2O3 aq. solution. The layers were separated and the organic washed with brine, dried (MgSO4), and concentrated in vacuo to provide the title compound as a solid (10.8 g).
後処理
- temperaturecooled to room temperature
- concentrationThe reaction mixture was concentrated in vacuo
- custompartitioned between CH2Cl2 and 2 M Na2S2O3 aq. solution
- customThe layers were separated
- washthe organic washed with brine
- dry with materialdried (MgSO4)
- concentrationconcentrated in vacuo
出典と根拠
- ORDレコード
- ord-e0a58e14d88c4772b337fbad60fd3375
- 出典データセット
- uspto-grants-2016_01
- 特許番号
- US09227976B2
反応ノート
読み込み中…