Ethanol → Ethyl 4-hydroxy-3-methoxy-5-nitrophenylglyoxylate

HRID 274456

反応式

HRID 274456 の反応式
Br[CH2:2][C:3]([C:5]1[CH:10]=[C:9]([N+:11]([O-:13])=[O:12])[C:8]([OH:14])=[C:7]([O:15][CH3:16])[CH:6]=1)=[O:4].[Se](=O)=[O:18].[CH2:20]([OH:22])[CH3:21]>>[OH:14][C:8]1[C:9]([N+:11]([O-:13])=[O:12])=[CH:10][C:5]([C:3](=[O:4])[C:2]([O:22][CH2:20][CH3:21])=[O:18])=[CH:6][C:7]=1[O:15][CH3:16]

参加物

4

反応物 3

HCID 702EthanolHCID 24007Selenium DioxideHCID 144509832-Bromo-4'-hydroxy-3'-methoxy-5'-nitroacetophenone

生成物 1

HCID 14450984Ethyl 4-hydroxy-3-methoxy-5-nitrophenylglyoxylate

実験手順

ba) A suspension of 580.1 mg of 2-bromo-4'-hydroxy-3'-methoxy-5'-nitroacetophenone in 10 ml of ethanol is treated with 443.8 mg of selenium dioxide and heated under reflux for 71 hours. Thereafter, the selenium is removed by filtration and the filtrate is evaporated. The residue is dissolved in methylene chloride, washed with saturated sodium chloride solution, dried over sodium sulfate, filtered and evaporated. There is obtained ethyl 4-hydroxy-3-methoxy-5-nitrophenylglyoxylate of m.p. 165°-167° (from ethanol).

後処理

  1. temperatureheated
  2. temperatureunder reflux for 71 hours
  3. customThereafter, the selenium is removed by filtration
  4. customthe filtrate is evaporated
  5. dissolutionThe residue is dissolved in methylene chloride
  6. washwashed with saturated sodium chloride solution
  7. dry with materialdried over sodium sulfate
  8. filtrationfiltered
  9. customevaporated

出典と根拠

ORDレコード
ord-845f99f42fd34254975aa45c54b5624e
出典データセット
uspto-grants-1995_02
特許番号
US05389653

関連ノート

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