1,3-Dioxolane-2-propylamine → 3-(3-[1,3]Dioxolan-2-yl-propylamino)butyronitrile

HRID 888759

반응식

HRID 888759 반응식
[O:1]1[CH2:5][CH2:4][O:3][CH:2]1[CH2:6][CH2:7][CH2:8][NH2:9].[C:10](#[N:14])/[CH:11]=[CH:12]/[CH3:13]>C(OCC)(=O)C>[O:1]1[CH2:5][CH2:4][O:3][CH:2]1[CH2:6][CH2:7][CH2:8][NH:9][CH:12]([CH3:13])[CH2:11][C:10]#[N:14]

참가 물질

4

반응물 2

HCID 780991,3-Dioxolane-2-propylamineHCID 637921Crotononitrile

생성물 1

HCID 688630333-(3-[1,3]Dioxolan-2-yl-propylamino)butyronitrile수율 92.6%

시약·촉매·용매 1

HCID 8857Ethyl Acetate용매

반응 조건

온도
100 °C

실험 절차

49.85 g (0.38 mol) of 3-[1,3]-dioxolan-2-yl-propylamine and 43.34 g (0.646 mol) of crotono-nitrile are combined in a 200 ml round-bottomed flask and heated at 100° C. for 72 hours. After cooling, the brown mass is diluted with ethyl acetate and washed with water. The organic phase is dried over calcium carbonate and purified by filtration on silica gel (eluent: ethyl acetate). Evaporation of the solvent gives 69.8 g of 3-(3-[1,3]-dioxolan-2-yl-propylamino)butyronitrile as a reddish liquid which is used without further purification in the next stage.

후처리

  1. temperatureAfter cooling
  2. washwashed with water
  3. dry with materialThe organic phase is dried over calcium carbonate
  4. filtrationpurified by filtration on silica gel (eluent: ethyl acetate)
  5. customEvaporation of the solvent

출처 및 근거

ORD 기록
ord-b17d6a09186343188dcfe257dc075376
출처 데이터셋
uspto-grants-2012_08
특허 번호
US08252784B2

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