Lactonitrile → 2-(Diisopropylamino)propionitrile

HRID 374667

반응식

HRID 374667 반응식
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]

참가 물질

5

반응물 3

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

생성물 1

HCID 109972602-(Diisopropylamino)propionitrile수율 75%

시약·촉매·용매 1

HCID 3283Diethyl Ether용매

반응 조건

온도
51 °C

실험 절차

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) .

후처리

  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

출처 및 근거

ORD 기록
ord-c47826333e954a139ba74d6485ed7449
출처 데이터셋
uspto-grants-1996_01
특허 번호
US05481038

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