Carbon tetrabromide → 2-(Bromomethyl)-3-fluoropyridine
反応式
[F:1][C:2]1[C:3]([CH2:8]O)=[N:4][CH:5]=[CH:6][CH:7]=1.C1(P(C2C=CC=CC=2)C2C=CC=CC=2)C=CC=CC=1.[Br:29]C(Br)(Br)Br>ClCCl>[Br:29][CH2:8][C:3]1[C:2]([F:1])=[CH:7][CH:6]=[CH:5][N:4]=1参加物
5
実験手順
A solution of 285 mg (2.242 mmol) of (3-fluoropyridin-2-yl)methanol (CAS: 31181-79-0) in dry dichloromethane (9 ml) in an ice-water bath and under an argon atmosphere was admixed with 882 mg (3.36 mmol) of triphenylphosphine and 1.12 g (3.36 mmol) of tetrabromomethane. The reaction mixture was stirred at room temperature for 22 hours. The solvent was evaporated off and the residue was purified by flash chromatography using a prepacked silica gel cartridge (mobile phase: cyclohexane-ethyl acetate, gradient 15% to 30%), which gave 156 mg (11% yield, 98% pure) of the target compound.
後処理
- customThe solvent was evaporated off
- customthe residue was purified by flash chromatography
- customgave 156 mg (11% yield, 98% pure) of the target compound
出典と根拠
- ORDレコード
- ord-b06ad1c19c914f41ac70f024944e6878
- 出典データセット
- uspto-grants-2016_08
- 特許番号
- US09422285B2
反応ノート
読み込み中…