Ethanol → 4-Chloro-5-(ethylamino)-2-methylphenol

HRID 1110647노트

반응식

HRID 1110647 반응식
[Cl:1][C:2]1[C:7]([NH2:8])=[CH:6][C:5]([OH:9])=[C:4]([CH3:10])[CH:3]=1.[CH2:11](I)[CH3:12].C(=O)([O-])O.[Na+].C(O)C>O>[CH3:10][C:4]1[CH:3]=[C:2]([Cl:1])[C:7]([NH:8][CH2:11][CH3:12])=[CH:6][C:5]=1[OH:9]

참가 물질

6

실험 절차

A mixture of 3 g of 4-chloro-2-methyl-5-aminophenol (0.016 mol), 2.6 g of ethyliodide (0.017 mol), 1.35 g of sodium hydrogen carbonate (0.016 mol) and 30 ml of ethanol was refluxed for 7 hours. After cooling and dilution with 50 ml of water, the solution was neutralized with a sodium hydrogen carbonate solution and then extracted three times with 50 ml of ethylacetate. The extract was dried over sodium sulfate and concentrated to dryness. The residue was recrystallized from toluene. Beige crystals melting at 205° C. were obtained.

후처리

  1. temperaturewas refluxed for 7 hours
  2. temperatureAfter cooling
  3. extractionextracted three times with 50 ml of ethylacetate
  4. dry with materialThe extract was dried over sodium sulfate
  5. concentrationconcentrated to dryness
  6. customThe residue was recrystallized from toluene

출처 및 근거

ORD 기록
ord-e37002ee09054b418ccc239f6988a117
출처 데이터셋
uspto-grants-1990_12
특허 번호
US04976742

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