Water → 5-((2-Hydroxyethyl)amino)-1,3-benzodioxol

HRID 1266185노트

반응식

HRID 1266185 반응식
[C:1]([O-])(=[O:3])[CH3:2].[Na+].BrCCO.[CH2:10]1[O:19][C:18]2[CH:17]=[CH:16][C:14]([NH2:15])=[CH:13][C:12]=2[O:11]1.O>C(O)C>[CH2:10]1[O:19][C:18]2[CH:17]=[CH:16][C:14]([NH:15][CH2:2][CH2:1][OH:3])=[CH:13][C:12]=2[O:11]1

참가 물질

6

반응물 4

HCID 962WaterHCID 108982-BromoethanolHCID 843101,3-Benzodioxol-5-amineHCID 517045Sodium Acetate

생성물 1

HCID 1755935-((2-Hydroxyethyl)amino)-1,3-benzodioxol

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

27 mmol of sodium acetate and 15 mmol of 2-bromoethanol are added to 10 mmol of 3,4-methylenedioxyaniline dissolved in ethanol. After 24 hours of heating at reflux, the reaction mixture is brought to ambient temperature, water is added, and then the aqueous phase is extracted with dichloromethane. The organic phases are combined, the solvent is evaporated off and the crude residue is purified by chromatography on silica, using a 10:90 dichloromethane/ethyl acetate mixture as eluant, to yield the expected product in the form of an oil.

후처리

  1. temperatureAfter 24 hours of heating
  2. temperatureat reflux
  3. customis brought to ambient temperature
  4. extractionthe aqueous phase is extracted with dichloromethane
  5. customthe solvent is evaporated off
  6. customthe crude residue is purified by chromatography on silica

출처 및 근거

ORD 기록
ord-056317faa3c64e5daee10c4e9c0514f7
출처 데이터셋
uspto-grants-2003_04
특허 번호
US06548515B1

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