Water → 2,6-Dichloro-4-nitrophenol

HRID 844291

반응식

HRID 844291 반응식
[Cl:1][C:2]1[CH:3]=[C:4]([N+:10]([O-:12])=[O:11])[CH:5]=[C:6]([Cl:9])[C:7]=1Cl.[O-:13]C1C=CC=CC=1.[K+].O>C(O)COCCO>[Cl:1][C:2]1[CH:3]=[C:4]([N+:10]([O-:12])=[O:11])[CH:5]=[C:6]([Cl:9])[C:7]=1[OH:13]

참가 물질

5

반응물 3

HCID 962WaterHCID 883653,4,5-TrichloronitrobenzeneHCID 23670670Potassium phenoxide

생성물 1

HCID 120662,6-Dichloro-4-nitrophenol

시약·촉매·용매 1

HCID 8117Diethylene Glycol용매

반응 조건

온도
160 °C

실험 절차

3,4,5-Trichloronitrobenzene (14.86 g) is added to a solution of potassium phenoxide (8.66 g) in diethylene glycol (66 mL) and the mixture is heated to 160° C. for approximately 15 hours. The resulting dark brown solution is cooled to room temperature, poured onto 100 mL cold water, and extracted twice with diethyl ether. The pooled organic extracts are washed with water, 10% aqueous sodium hydroxide, and then dried over anhydrous magnesium sulfate. Following removal of the solvent under reduced pressure the resulting oil is distilled in a Kugelrohr apparatus to provide a yellow oil that solidifies on standing. Recrystallization from ethanol-water provides the desired product as a pale yellow solid.

후처리

  1. temperatureThe resulting dark brown solution is cooled to room temperature
  2. extractionextracted twice with diethyl ether
  3. washThe pooled organic extracts are washed with water, 10% aqueous sodium hydroxide
  4. dry with materialdried over anhydrous magnesium sulfate
  5. customremoval of the solvent under reduced pressure the resulting oil
  6. distillationis distilled in a Kugelrohr apparatus
  7. customto provide a yellow oil
  8. customRecrystallization from ethanol-water

출처 및 근거

ORD 기록
ord-0c1aba098055454997a54beef0b5fa3a
출처 데이터셋
uspto-grants-2002_04
특허 번호
US06380243B1

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