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Hydrochloric Acid → N-Methyl-N-[2-(3,4-dimethoxyphenyl)ethyl]-2-methyl-1,3-propanediamine

HRID 974996
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반응식

HRID 974996 반응식
[CH3:1][N:2]([CH2:15][CH:16]([CH3:19])[C:17]#[N:18])[CH2:3][CH2:4][C:5]1[CH:10]=[CH:9][C:8]([O:11][CH3:12])=[C:7]([O:13][CH3:14])[CH:6]=1.Cl>C(O)C.[Pt]=O>[CH3:1][N:2]([CH2:3][CH2:4][C:5]1[CH:10]=[CH:9][C:8]([O:11][CH3:12])=[C:7]([O:13][CH3:14])[CH:6]=1)[CH2:15][CH:16]([CH3:19])[CH2:17][NH2:18]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 2

HCID 313Hydrochloric AcidHCID 199703153-[N-methyl-N-(2-(3,4-dimethoxyphenyl)ethyl)amino]-2-methylpropionitrile

생성물 1

HCID 15045284N-Methyl-N-[2-(3,4-dimethoxyphenyl)ethyl]-2-methyl-1,3-propanediamine수율 92.9%

시약·촉매·용매 2

HCID 82844Platinum oxide (PtO)촉매HCID 702Ethanol용매

실험 절차

2.1 g of the above nitrile and 0.2 ml of concentrated hydrochloric acid were dissolved in 30 ml of ethanol, followed by the addition of 0.2 g of platinum oxide to carry out hydrogenation under a hydrogen pressure of 2.1 kg/cm2. The reaction mixture was filtered to remove the catalyst. The filtrate was distilled under a reduced pressure to remove the ethanol. The residue was made alkaline with a dilute solution of caustic soda. The aqueous layer was extracted with dichloromethane. The extract was washed with water, dried over magnesium sulfate and distilled under a reduced pressure to obtain 1.98 g of the title compound as a pale yellow oil (yield: 38%).

후처리

  1. filtrationThe reaction mixture was filtered
  2. customto remove the catalyst
  3. distillationThe filtrate was distilled under a reduced pressure
  4. customto remove the ethanol
  5. extractionThe aqueous layer was extracted with dichloromethane
  6. washThe extract was washed with water
  7. dry with materialdried over magnesium sulfate
  8. distillationdistilled under a reduced pressure

출처 및 근거

ORD 기록
ord-b9ec535add8c4572b16755b419caa99a
출처 데이터셋
uspto-grants-1997_03
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05607953

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