4,5-Dichloro-2-nitrophenol → 2-Amino-4,5-dichlorophenol

HRID 588767

반응식

HRID 588767 반응식
[Cl:1][C:2]1[C:7]([Cl:8])=[CH:6][C:5]([OH:9])=[C:4]([N+:10]([O-])=O)[CH:3]=1>C(O)(=O)C.O.[Fe]>[NH2:10][C:4]1[CH:3]=[C:2]([Cl:1])[C:7]([Cl:8])=[CH:6][C:5]=1[OH:9]

참가 물질

5

반응물 1

HCID 382484,5-Dichloro-2-nitrophenol

생성물 1

HCID 30154152-Amino-4,5-dichlorophenol수율 78%

시약·촉매·용매 3

HCID 23925Iron촉매HCID 176Acetic Acid용매HCID 962Water용매

반응 조건

온도
50 °C

실험 절차

To a stirred solution of 4,5-dichloro-2-nitrophenol (15 g, 72 mmol) in acetic acid (150 mL) and water (450 mL), iron powder (16 g, 285 mmol) was added in portions. The resulting mixture was stirred at 50° C. for 2 h. The mixture was allowed to cool to room temperature, filtered, and the cake was rinsed with ethyl acetate. The filtrate was extracted with ethyl acetate. The organic layer was washed with water, NaHCO3 (aq.) and brine, dried over Na2SO4 and concentrated in vacuo to afford the desired product (10 g, 78%).

후처리

  1. temperatureto cool to room temperature
  2. filtrationfiltered
  3. washthe cake was rinsed with ethyl acetate
  4. extractionThe filtrate was extracted with ethyl acetate
  5. washThe organic layer was washed with water, NaHCO3 (aq.) and brine
  6. dry with materialdried over Na2SO4
  7. concentrationconcentrated in vacuo

출처 및 근거

ORD 기록
ord-bff78745c1124b84b578a242800471d8
출처 데이터셋
uspto-grants-2016_01
특허 번호
US09227978B2

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