Carbon Tetrachloride → 2-(1-Chloroethyl)-5-fluoropyridine
反応式
C1(P(C2C=CC=CC=2)C2C=CC=CC=2)C=CC=CC=1.C(Cl)(Cl)(Cl)[Cl:21].[F:25][C:26]1[CH:27]=[CH:28][C:29]([CH:32](O)[CH3:33])=[N:30][CH:31]=1.CCCCC>C(Cl)Cl>[Cl:21][CH:32]([C:29]1[CH:28]=[CH:27][C:26]([F:25])=[CH:31][N:30]=1)[CH3:33]参加物
6
実験手順
A mixture of triphenylphospine (0.92 g, 3.5 mmol) and CCl4 (4 mL) was stirred for 10 min. and then a solution of 1-(5-fluoropyridin-2-yl)ethanol (0.25 g, 1.7 mmol) in DCM (2 mL) was added. After 18 h, pentane (20 mL) was added, the solid material was removed by filtration and the filtrate was concentrated in vacuo. The residue was purified by flash column chromatography (eluent heptane:ethyl acetate 3:1) affording the title compound (8 mg, 3% yield).
後処理
- waitAfter 18 h
- customthe solid material was removed by filtration
- concentrationthe filtrate was concentrated in vacuo
- customThe residue was purified by flash column chromatography (eluent heptane:ethyl acetate 3:1)
出典と根拠
- ORDレコード
- ord-af6820bd0fc746cd96180bbe93fcc51e
- 出典データセット
- uspto-grants-2012_04
- 特許番号
- US08158785B2
反応ノート
読み込み中…