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

HRID 274456

반응식

HRID 274456 반응식
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]

참가 물질

4

반응물 3

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

생성물 1

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

실험 절차

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).

후처리

  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

출처 및 근거

ORD 기록
ord-845f99f42fd34254975aa45c54b5624e
출처 데이터셋
uspto-grants-1995_02
특허 번호
US05389653

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