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

HRID 1073765노트

반응식

HRID 1073765 반응식
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]

참가 물질

4

반응물 2

HCID 8902DipropylamineHCID 221567582-(Chloromethyl)piperidine hydrochloride

생성물 1

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

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

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).

후처리

  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

출처 및 근거

ORD 기록
ord-08459017514b478dba3daa5a6216b4d9
출처 데이터셋
uspto-grants-1990_11
특허 번호
US04971966

반응 노트

불러오는 중…