N-bromobutanimide → N-(4-bromo-2-(bromomethyl)phenyl)-2,2,2-trifluoroacetamide
反応式
[Br:1][C:2]1[CH:7]=[CH:6][C:5]([NH:8][C:9](=[O:14])[C:10]([F:13])([F:12])[F:11])=[C:4]([CH3:15])[CH:3]=1.[Br:16]N1C(=O)CCC1=O>C(Cl)(Cl)(Cl)Cl>[Br:1][C:2]1[CH:7]=[CH:6][C:5]([NH:8][C:9](=[O:14])[C:10]([F:12])([F:13])[F:11])=[C:4]([CH2:15][Br:16])[CH:3]=1参加物
4
実験手順
A solution of Example 478A (2.5 g, 8.9 mmol) and N-bromosuccinimide (1.58 g, 8.9 mmol) in carbon tetrachloride (25 mL) was irradiated with a 100-watt incandescent bulb overnight. The solution was filtered and the filtrate was concentrated. The concentrate was purified by flash chromatography on silica gel using 3-4% ethyl acetate/hexanes to give 2.17 g (68% yield) of the desired product. MS (ESI(−)) m/e 360, 362 (M−H)−.
後処理
- filtrationThe solution was filtered
- concentrationthe filtrate was concentrated
- customThe concentrate was purified by flash chromatography on silica gel using 3-4% ethyl acetate/hexanes
出典と根拠
- ORDレコード
- ord-bc163b3b6c5043ce898c1c3e4a55dac4
- 出典データセット
- uspto-grants-2012_09
- 特許番号
- US08273736B2
反応ノート
読み込み中…