Water → 1-Bromo-3-(bromomethyl)-4-chloro-2-fluorobenzene
反応式
P(Br)(Br)[Br:2].[Br:5][C:6]1[C:7]([F:15])=[C:8]([CH2:13]O)[C:9]([Cl:12])=[CH:10][CH:11]=1.O>ClCCl>[Br:5][C:6]1[CH:11]=[CH:10][C:9]([Cl:12])=[C:8]([CH2:13][Br:2])[C:7]=1[F:15]参加物
5
実験手順
Add phosphorous tribromide (1.8 mL, 19.2 mmol) to (3-bromo-6-chloro-2-fluoro-phenyl)methanol (Preparation 8) (4.6 g, 19 mmol) in dichloromethane (50 mL) at 0° C. Stir for 20 minutes. Add the reaction mixture into ice and water. Extract with dichloromethane (100 mL), dry with magnesium sulfate, filter and evaporate solvent under reduced pressure. Purify the residue by biotage chromatography to yield the product to give 1.7 g (30%) of the title compound as a white solid. 1HNMR (CDCl3) 7.48-7.44 (m, 1H), 7.14-7.11 (m, 1H), 4.62-4.61(m, 2H).
後処理
- extractionExtract with dichloromethane (100 mL)
- dry with materialdry with magnesium sulfate
- filtrationfilter
- customevaporate solvent under reduced pressure
- customPurify the residue by biotage chromatography
- customto yield the product
出典と根拠
- ORDレコード
- ord-ba88538709ef4fb6b226b3518c7d47d3
- 出典データセット
- uspto-grants-2010_05
- 特許番号
- US07713979B2
反応ノート
読み込み中…