Dipropylamine → N-(Piperidin-2-ylmethyl)-N-propylpropan-1-amine

HRID 1073765ノート

反応式

HRID 1073765 の反応式
Cl.Cl[CH2:3][CH:4]1[CH2:9][CH2:8][CH2:7][CH2:6][NH:5]1.[CH2:10]([NH:13][CH2:14][CH2:15][CH3:16])[CH2:11][CH3:12]>ClCCl>[CH2:10]([N:13]([CH2:3][CH:4]1[CH2:9][CH2:8][CH2:7][CH2:6][NH:5]1)[CH2:14][CH2:15][CH3:16])[CH2:11][CH3:12]

参加物

4

反応物 2

HCID 8902DipropylamineHCID 221567582-(Chloromethyl)piperidine hydrochloride

生成物 1

HCID 10798040N-(Piperidin-2-ylmethyl)-N-propylpropan-1-amine

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

A mixture of 170.1 g (1.0 mole) of 2-(chloromethyl)piperidine hydrochloride (M. Rink and H. G. Liem, Arch. Pharm. 292, 165-169 (1959)), 506 g (5.0 mole) of dipropylamine and 1.7 1 of dichloromethane were boiled under reflux for 3 hours, then evaporated in vacuo, and the residue was made alkaline with potassium hydroxide solution with external ice cooling. Exhaustive extraction with t-butyl methyl ether was carried out, and the combined extracts were washed twice with 100 ml of water each time, dried over sodium sulphate, and the solvent was removed by distillation in vacuo. The residue was fractionally distilled under water pump vacuum. Colourless oil of boiling point 108-114° C. (12 mm Hg ). Yield: 108.6 g (55% of theory).

後処理

  1. temperatureunder reflux for 3 hours
  2. customevaporated in vacuo
  3. extractionExhaustive extraction with t-butyl methyl ether
  4. washthe combined extracts were washed twice with 100 ml of water each time
  5. dry with materialdried over sodium sulphate
  6. customthe solvent was removed by distillation in vacuo
  7. distillationThe residue was fractionally distilled under water

出典と根拠

ORDレコード
ord-08459017514b478dba3daa5a6216b4d9
出典データセット
uspto-grants-1990_11
特許番号
US04971966

反応ノート

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