Lactonitrile → 2-(Diisopropylamino)propionitrile

HRID 374667

反応式

HRID 374667 の反応式
S([O-])([O-])(=O)=O.[Mg+2].[CH:7]([NH:10][CH:11]([CH3:13])[CH3:12])([CH3:9])[CH3:8].[C:14](#[N:18])[CH:15]([CH3:17])O>C(OCC)C>[CH:7]([N:10]([CH:11]([CH3:13])[CH3:12])[CH:15]([CH3:17])[C:14]#[N:18])([CH3:9])[CH3:8]

参加物

5

反応物 3

HCID 6572LactonitrileHCID 7912DiisopropylamineHCID 24083Sulfuric acid magnesium salt (1:1)

生成物 1

HCID 109972602-(Diisopropylamino)propionitrile収率 75%

試薬・触媒・溶媒 1

HCID 3283Diethyl Ether溶媒

反応条件

温度
51 °C

実験手順

Anhydrous magnesium sulfate (12.04 g, 0.1 mol) was added to diisopropylamine (12.14 g, 0.12 mol), followed by lactonitrile (7.73 g of 92% aqueous solution, 0.1 mol) added all at once with stirring. The reaction mixture spontaneously warmed up to 51° C. It was left overnight at room temperature. Diethyl ether (50 ml) was added, and magnesium sulfate was filtered off and washed with ether (50 ml). The product was isolated by distillation, 11.57 g, 75% yield, bp 49°-50° C./0.1 mm Hg. 1H NMR CDCl3 δ ppm, 1.02 (d, J=6.5 Hz, 6H, CH3), 1.17 (d, J=6.5 Hz, 6H, CH3), 1.41 (d, J=6.5 Hz, 3H, CH3, 3.21 (sep, J=6.5 Hz, 2H,=CH) , 3.89 (q, J=6.5 Hz, 1H, CH) .

後処理

  1. additionadded all at once
  2. filtrationmagnesium sulfate was filtered off
  3. washwashed with ether (50 ml)
  4. customThe product was isolated by distillation, 11.57 g, 75% yield, bp 49°-50° C./0.1 mm Hg

出典と根拠

ORDレコード
ord-c47826333e954a139ba74d6485ed7449
出典データセット
uspto-grants-1996_01
特許番号
US05481038

関連ノート

読み込み中…