N,N-Dimethylaniline → HCID 11992622, 화합물

HRID 420826노트

반응식

HRID 420826 반응식
[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

참가 물질

5

반응물 3

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

생성물 1

HCID 11992622HCID 11992622, 화합물

시약·촉매·용매 1

HCID 8857Ethyl Acetate용매

실험 절차

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.

후처리

  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)

출처 및 근거

ORD 기록
ord-9bd8df5a8036493ab4bbe05e081921d1
출처 데이터셋
uspto-grants-2012_01
특허 번호
US08097656B2

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