反応式
[Cl:1][C:2]1[CH:7]=C(C#N)[CH:5]=[CH:4][N:3]=1.[CH3:10][Mg]Cl.Cl.C([O:16][CH2:17][CH3:18])C>>[C:17]([C:18]1[CH:5]=[CH:4][N:3]=[C:2]([Cl:1])[CH:7]=1)(=[O:16])[CH3:10]参加物
5
実験手順
24.61 g (177.62 mmol) of 2-chloro-4-cyano-pyridine are placed in 1.25 litres of diethyl ether under nitrogen, and 120 ml (22% in tetrahydrofuran, 353 mmol) of methyl-magnesium chloride are added. The red suspension is stirred for 40 h at RT, poured onto 1.25 litres of ice/water and 250 ml of 6N HCl and stirred for 14 h at RT. Extraction with diethyl ether and methylene chloride, drying with MgSO4 and concentration give 4-acetyl-2-chloro-pyridine; Rf =0.5 (methylene chloride:methanol=9:1).
後処理
- stirringstirred for 14 h at RT
- extractionExtraction with diethyl ether and methylene chloride
- dry with materialdrying with MgSO4 and concentration
出典と根拠
- ORDレコード
- ord-160c9a75cc8c48d189fa78e2f7af0bda
- 出典データセット
- uspto-grants-1998_03
- 特許番号
- US05728708
関連ノート
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