Water → 1,3-Dioxolane-2-propylamine

HRID 888758

반응식

HRID 888758 반응식
[H-].[Al+3].[Li+].[H-].[H-].[H-].[O:7]1[CH2:11][CH2:10][O:9][CH:8]1[CH2:12][CH2:13][C:14]#[N:15].O.[OH-].[Na+]>CCOCC>[O:7]1[CH2:11][CH2:10][O:9][CH:8]1[CH2:12][CH2:13][CH2:14][NH2:15]

참가 물질

6

반응물 4

HCID 962Water2회HCID 14798Sodium HydroxideHCID 780981,3-Dioxolane-2-propiononitrileHCID 21226445Aluminium lithium hydride

생성물 1

HCID 780991,3-Dioxolane-2-propylamine

시약·촉매·용매 1

HCID 3283Diethyl Ether용매

실험 절차

50.1 g (1.32 mol) of lithium aluminium hydride are suspended in 500 ml of ether. Added dropwise to this suspension is a solution of 111.9 g (0.88 mol) of 3-[1,3]-dioxolan-2-yl-propionitrile. The mixture is subsequently heated at reflux for 2.5 hours. After cooling, 50 g of water, 50 g of 10% strength sodium hydroxide solution and a further 150 g of water are added. The mixture is then filtered and the filtrate is dried over calcium chloride and concentrated. The orange oil obtained is subsequently distilled under reduced pressure (overhead temperature=46° C., p=0.016 mbar). This gives 68.4 g of 3-[1,3]-dioxolan-2-yl-propylamine.

후처리

  1. additionAdded dropwise to this suspension
  2. temperatureThe mixture is subsequently heated
  3. temperatureat reflux for 2.5 hours
  4. temperatureAfter cooling
  5. filtrationThe mixture is then filtered
  6. dry with materialthe filtrate is dried over calcium chloride
  7. concentrationconcentrated
  8. customThe orange oil obtained
  9. distillationis subsequently distilled under reduced pressure (overhead temperature=46° C., p=0.016 mbar)

출처 및 근거

ORD 기록
ord-4e06467f95b147448eeea66ea72a1316
출처 데이터셋
uspto-grants-2012_08
특허 번호
US08252784B2

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