Tetrahydrofuran → 1-(6-Chloropyridin-2-yl)ethanone
反応式
[Cl:1][C:2]1[CH:7]=CC=C(C#N)[N:3]=1.[CH3:10][Mg]I.[CH2:13]1[CH2:17][O:16][CH2:15][CH2:14]1>C(OCC)C>[Cl:1][C:2]1[CH:7]=[CH:15][CH:14]=[C:13]([C:17](=[O:16])[CH3:10])[N:3]=1参加物
5
実験手順
A solution of 2-chloro-6-cyanopyridine (50 g) in THF (400 ml) is cooled to −5° C. and a solution of methylmagnesium iodide in diethyl ether (3 M, 200 ml) is added. After 1 h at 0° C. the ether is destilled off and the THF-mixture is heated to 60° C. for 1 h. The THF is evaporated and the residue is treated with ice water and acidified with 2 M hydrochloric acid. The water phase is extracted with dichloromethane and after drying and evaporation of the organic phase, the residue is purified by silica-gel flash chromatography. The title compound is obtained as an oil (11.2 g).
後処理
- customThe THF is evaporated
- additionthe residue is treated with ice water
- extractionThe water phase is extracted with dichloromethane
- customafter drying
- customevaporation of the organic phase
- customthe residue is purified by silica-gel flash chromatography
出典と根拠
- ORDレコード
- ord-e9a636cca3c340d69cd851d12531c500
- 出典データセット
- uspto-grants-2003_03
- 特許番号
- US06528456B2
反応ノート
読み込み中…