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

HRID 1266185ノート

反応式

HRID 1266185 の反応式
[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

参加物

6

反応物 4

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-056317faa3c64e5daee10c4e9c0514f7
出典データセット
uspto-grants-2003_04
特許番号
US06548515B1

反応ノート

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