Water → 1,3-Dioxolane-2-propylamine

HRID 888758ノート

反応式

HRID 888758 の反応式
[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]

参加物

6

反応物 4

HCID 962Water2 回HCID 14798Sodium HydroxideHCID 780981,3-Dioxolane-2-propiononitrileHCID 21226445Aluminium lithium hydride

生成物 1

HCID 780991,3-Dioxolane-2-propylamine

試薬・触媒・溶媒 1

HCID 3283Diethyl Ether溶媒

実験手順

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.

後処理

  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)

出典と根拠

ORDレコード
ord-4e06467f95b147448eeea66ea72a1316
出典データセット
uspto-grants-2012_08
特許番号
US08252784B2

反応ノート

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