Ammonia → 2-[4-(Aminomethyl)phenoxy]-N,N-diethylethan-1-amine

HRID 215754

반응식

HRID 215754 반응식
[CH2:1]([N:3]([CH2:6][CH2:7][O:8][C:9]1[CH:16]=[CH:15][C:12]([CH:13]=O)=[CH:11][CH:10]=1)[CH2:4][CH3:5])[CH3:2].[NH3:17]>C(O)C.[Ni]>[CH2:1]([N:3]([CH2:6][CH2:7][O:8][C:9]1[CH:16]=[CH:15][C:12]([CH2:13][NH2:17])=[CH:11][CH:10]=1)[CH2:4][CH3:5])[CH3:2]

참가 물질

5

반응물 2

HCID 222AmmoniaHCID 4116744-(2-(Diethylamino)-Ethoxy)-Benzaldehyde

생성물 1

HCID 2359442-[4-(Aminomethyl)phenoxy]-N,N-diethylethan-1-amine수율 65%

시약·촉매·용매 2

HCID 935Nickel촉매HCID 702Ethanol용매

반응 조건

온도
80 °C

실험 절차

To the solution of 4-diethylaminoethoxybenzaldehyde X in 180 ml 10% solution of ammonia in anhydrous ethanol, 4.5 g RaNi was added and the mixture was heated to 80° C. at the pressure 68 atm in the autoclave under hydrogen input to the reaction mixture under stirring for 12 hours. The mixture was cooled, the catalyst was filtered off, washed with ethanol. The solvent was distilled off from the solution and the distillation residue was purified by distillation under the reduced pressure. Afforded 13 g (65%) of 4-diethylaminoethoxybenzylamine XI. Colourless fluid 138-140° C./0.5 torr, n20D=1.520. Lit. [6.7] reports 130° C./0.3 torr, n20D=1.5220.

후처리

  1. temperatureThe mixture was cooled
  2. filtrationthe catalyst was filtered off
  3. washwashed with ethanol
  4. distillationThe solvent was distilled off from the solution
  5. distillationthe distillation residue was purified by distillation under the reduced pressure

출처 및 근거

ORD 기록
ord-854c51b8d09f40c48d3a03ca81d923d3
출처 데이터셋
uspto-grants-2012_06
특허 번호
US08193184B2

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