2,5-Dichlorophenol → 2,5-Dichloro-4-nitrophenol

HRID 1957470

반응식

HRID 1957470 반응식
[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([Cl:8])=[CH:4][C:3]=1[OH:9].[N+:10]([O-])([OH:12])=[O:11]>ClCCl>[Cl:1][C:2]1[CH:7]=[C:6]([N+:10]([O-:12])=[O:11])[C:5]([Cl:8])=[CH:4][C:3]=1[OH:9]

참가 물질

4

반응물 2

HCID 662,5-DichlorophenolHCID 944Nitric Acid

생성물 1

HCID 221082,5-Dichloro-4-nitrophenol수율 31%

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

2,5-dichlorophenol (72 g, 440 mmol) were slurried in 100 ml dichloromethane which resulted in an endothermic reaction. To this mixture were slowly added 30 ml (480 mmol) concentrated nitric acid. The reaction was allowed to reach and maintain reflux. The mixture was stirred until it reached ambient temperature and all materials remained in solution. 50 g of ice were added and solids precipitated. The mixture was filtered cold and washed with 25 ml dichloromethane, 50 ml dichloromethane, then twice with 25 ml dichloromethane to yield 28.4 g of 2,5-dichloro-4-nitrophenol.

후처리

  1. customresulted in an endothermic reaction
  2. temperaturemaintain
  3. temperaturereflux
  4. customreached ambient temperature
  5. customsolids precipitated
  6. filtrationThe mixture was filtered cold
  7. washwashed with 25 ml dichloromethane, 50 ml dichloromethane

출처 및 근거

ORD 기록
ord-dac27d0877c748b2bf7ed384d762bcf7
출처 데이터셋
uspto-grants-1998_07
특허 번호
US05786301

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