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

HRID 493906ノート

反応式

HRID 493906 の反応式
[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]

参加物

4

反応物 2

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 8857Ethyl Acetate溶媒

反応条件

温度
100 °C

実験手順

49.85 g (0.38 mol) of 3-[1,3]-dioxolan-2-yl-propylamine and 43.34 g (0.646 mol) of crotononitrile 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-ylpropylamino)butyronitrile as a reddish liquid which is used without further purification in the next stage.

後処理

  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

出典と根拠

ORDレコード
ord-260fc75e9e3940c4bf0fe6592cab4abd
出典データセット
uspto-grants-2009_05
特許番号
US07538104B2

反応ノート

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