N,N-Dimethylaniline → HCID 11992622、化合物

HRID 420826ノート

反応式

HRID 420826 の反応式
[CH3:1][O:2][C:3]1[CH:4]=[C:5]([CH:7]=[C:8]([O:10][CH3:11])[CH:9]=1)[NH2:6].Br[CH2:13][C:14]([C:16]1[CH:21]=[C:20]([O:22][CH3:23])[CH:19]=[C:18]([O:24][CH3:25])[CH:17]=1)=O.CN(C)C1C=CC=CC=1>CCOC(C)=O>[CH3:11][O:10][C:8]1[CH:9]=[C:3]([O:2][CH3:1])[CH:4]=[C:5]2[C:7]=1[CH:13]=[C:14]([C:16]1[CH:17]=[C:18]([O:24][CH3:25])[CH:19]=[C:20]([O:22][CH3:23])[CH:21]=1)[NH:6]2

参加物

5

反応物 3

HCID 949N,N-DimethylanilineHCID 663013,5-DimethoxyanilineHCID 27569322-Bromo-1-(3,5-dimethoxyphenyl)ethanone

生成物 1

HCID 11992622HCID 11992622、化合物

試薬・触媒・溶媒 1

HCID 8857Ethyl Acetate溶媒

実験手順

0.32 g (2.1 mmoles) of 3,5-dimethoxyaniline, 0.26 g (1.0 mmol) of 2-bromo-1-(3,5-dimethoxyphenyl)ethanone and 0.42 ml (3.3 mmol) of N,N-dimethylaniline were placed in a vial. The vial was placed inside a monomode microwave reactor and was radiated at a power of 100 W, at a temperature of 150° C. for 10 minutes. After cooling the reaction vial, the mixture was dissolved in AcOEt, was washed with an aqueous HCl 2N solution, was dried on anhydrous Na2SO4 and was evaporated at low pressure. The crude portion was purified by means of pressure column chromatography (Eluent: AcOEt/hexanes) obtaining 4,6-dimethoxy-2-(3,5-dimethoxyphenyl)-1H-indole.

後処理

  1. customThe vial was placed inside a monomode microwave reactor
  2. temperatureAfter cooling the reaction vial, the mixture
  3. washwas washed with an aqueous HCl 2N solution
  4. dry with materialwas dried on anhydrous Na2SO4
  5. customwas evaporated at low pressure
  6. customThe crude portion was purified by means of pressure column chromatography (Eluent: AcOEt/hexanes)

出典と根拠

ORDレコード
ord-9bd8df5a8036493ab4bbe05e081921d1
出典データセット
uspto-grants-2012_01
特許番号
US08097656B2

反応ノート

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