Ethyl Bromide → 3-ethoxy-N-ethyl-4-nitrobenzamide

HRID 1717281ノート

反応式

HRID 1717281 の反応式
[CH2:1]([NH:3][C:4](=[O:15])[C:5]1[CH:10]=[CH:9][C:8]([N+:11]([O-:13])=[O:12])=[C:7]([OH:14])[CH:6]=1)[CH3:2].C(=O)([O-])[O-].[K+].[K+].Br[CH2:23][CH3:24]>CC(C)=O>[CH2:23]([O:14][C:7]1[CH:6]=[C:5]([CH:10]=[CH:9][C:8]=1[N+:11]([O-:13])=[O:12])[C:4]([NH:3][CH2:1][CH3:2])=[O:15])[CH3:24]

参加物

5

反応物 3

HCID 6332Ethyl BromideHCID 11430Potassium CarbonateHCID 21029708N-ethyl-3-hydroxy-4-nitrobenzamide

生成物 1

HCID 685151263-ethoxy-N-ethyl-4-nitrobenzamide収率 30%

試薬・触媒・溶媒 1

HCID 180Acetone溶媒

実験手順

To a solution of N-ethyl-3-hydroxy-4-nitrobenzamide (2.1 g) obtained in Example 74a) in acetone (100 ml) were added potassium carbonate (1.4 g) and bromoethane (0.75 ml), and the mixture was heated under reflux overnight. After cooling to room temperature, the solvent was evaporated under reduced pressure. Water and ethyl acetate were added to the residue, and the organic layer was fractionated. The organic layer was dried over sodium sulfate, and the solvent was evaporated under reduced pressure to give the title compound as a pale-brown solid (0.72 g, 30%).

後処理

  1. temperaturethe mixture was heated
  2. temperatureunder reflux overnight
  3. customthe solvent was evaporated under reduced pressure
  4. additionWater and ethyl acetate were added to the residue
  5. dry with materialThe organic layer was dried over sodium sulfate
  6. customthe solvent was evaporated under reduced pressure

出典と根拠

ORDレコード
ord-647b9f725cd9433cbdf87cf08bbe8569
出典データセット
uspto-grants-2010_09
特許番号
US07803822B2

反応ノート

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