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Triethylamine → 3-[N-methyl-N-(2-(3,4-dimethoxyphenyl)ethyl)amino]-2-methylpropionitrile

HRID 728051
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인쇄 미리보기

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HRID 728051 반응식
I.[CH3:2][NH:3][CH2:4][CH2:5][C:6]1[CH:11]=[CH:10][C:9]([O:12][CH3:13])=[C:8]([O:14][CH3:15])[CH:7]=1.[C:16](#[N:20])[C:17]([CH3:19])=[CH2:18].C(N(CC)CC)C>ClCCl>[CH3:2][N:3]([CH2:18][CH:17]([CH3:19])[C:16]#[N:20])[CH2:4][CH2:5][C:6]1[CH:11]=[CH:10][C:9]([O:12][CH3:13])=[C:8]([O:14][CH3:15])[CH:7]=1
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참가 물질

5

반응물 3

HCID 8471TriethylamineHCID 31368MethacrylonitrileHCID 44144798(3,4-Dimethoxyphenethyl)(methyl)ammonium iodide

생성물 1

HCID 199703153-[N-methyl-N-(2-(3,4-dimethoxyphenyl)ethyl)amino]-2-methylpropionitrile수율 39.8%

시약·촉매·용매 1

HCID 6344Dichloromethane용매

반응 조건

온도
70 °C

실험 절차

A mixture comprising 6.5 g of N-methyl-2-(3,4-dimethoxyphenyl)ethylamine hydroiodide, 1.6 g of methacrylonitrile and 2.4 g of triethylamine was heated at about 70° C. for 2.5 hours and cooled, followed by the addition of dichloromethane. The obtained mixture was washed with water, dried over magnesium sulfate and distilled to remove the solvent. The residue was purified by silica gel column chromatography (solvent: dichloromethane/ethanol (100:1)) to obtain 2.1 g of 3-[N-methyl-N-(2-(3,4-dimethoxyphenyl)ethyl)-amino]-2-methylpropionitrile.

후처리

  1. temperaturecooled
  2. washThe obtained mixture was washed with water
  3. dry with materialdried over magnesium sulfate
  4. distillationdistilled
  5. customto remove the solvent
  6. customThe residue was purified by silica gel column chromatography (solvent: dichloromethane/ethanol (100:1))

출처 및 근거

ORD 기록
ord-61765b89637542e4bd93bf4173b012e6
출처 데이터셋
uspto-grants-1991_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05047417

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