反応式
[CH2:1]([Mg]Cl)[CH2:2][CH3:3].[CH3:6]COCC.[C:11]([C:13](=[CH:17][CH:18]([CH3:20])[CH3:19])[C:14]([OH:16])=[O:15])#[N:12]>C1COCC1>[CH3:6][O:15][C:14](=[O:16])[CH:13]([C:11]#[N:12])[CH:17]([CH:18]([CH3:20])[CH3:19])[CH2:1][CH2:2][CH3:3]参加物
5
反応条件
- 温度
- -40 °C
実験手順
A 2.0 M solution of propyl magnesium chloride in Et2O (9.8 mL, 19.6 mmol) is added to a solution of 2-cyano4-methyl-2-pentenoic acid (3.0 g, 19.6 mmol) in 50 mL of THF which is cooled in an IPA/dry ice bath to −40° C. under argon. The solution is stirred for 4 hours, and the reaction is quenched by addition of 50 mL of saturated KH2PO4. The THF is evaporated, and the remaining oil is chromatographed under medium pressure over silica gel with 50% CH2Cl2/hexane. Yield=1.9 g (50%) of 2-cyano-3-isopropyl-hexanoic acid methyl ester as an oil.
後処理
- customthe reaction is quenched by addition of 50 mL of saturated KH2PO4
- customThe THF is evaporated
- customthe remaining oil is chromatographed under medium pressure over silica gel with 50% CH2Cl2/hexane
出典と根拠
- ORDレコード
- ord-95663f39283f40eebdf4a2bdf8748c20
- 出典データセット
- uspto-grants-2003_11
- 特許番号
- US06642398B2
関連ノート
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