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

HRID 728051
ノート
印刷プレビュー

反応式

HRID 728051 の反応式
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
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

反応条件

温度
70 °C

実験手順

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.

後処理

  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))

出典と根拠

ORDレコード
ord-61765b89637542e4bd93bf4173b012e6
出典データセット
uspto-grants-1991_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05047417

反応ノート

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このページの内容参加物反応条件実験手順後処理出典と根拠反応ノート