Chlorosuccinimide → 935777-25-6
反応式
[F:1][C:2]([F:11])([F:10])[C:3]1[N:8]=[N:7][C:6]([NH2:9])=[CH:5][CH:4]=1.[Cl:12]N1C(=O)CCC1=O>C(#N)C>[Cl:12][C:5]1[CH:4]=[C:3]([C:2]([F:1])([F:10])[F:11])[N:8]=[N:7][C:6]=1[NH2:9]参加物
4
反応条件
- 温度
- 70 °C
実験手順
A mixture of D6 (4.0 g, 24.5 mmol) and N-chlorosuccinimide (3.3 g, 24.5 mmol) in acetonitrile (160 ml) was heated at 70° C. for 18 h. After this period, the reaction was cooled to room temperature and the solvents evaporated in vacuo. The crude residue was purified by column chromatography (silica; 3%-5% methanol/dichloromethane) to give D7 (1.6 g, 33%). C5H3ClF3N3 requires 197; Found 198 (MH+)
後処理
- waitAfter this period
- temperaturethe reaction was cooled to room temperature
- customthe solvents evaporated in vacuo
- customThe crude residue was purified by column chromatography (silica; 3%-5% methanol/dichloromethane)
出典と根拠
- ORDレコード
- ord-90b970214969402fb06786c7750dffe9
- 出典データセット
- uspto-grants-2015_01
- 特許番号
- US08940743B2
反応ノート
読み込み中…