Ammonium Chloride → 3-Bromo-5-fluoro-2-methylaniline

HRID 389663

반응식

HRID 389663 반응식
[Br:1][C:2]1[CH:7]=[C:6]([F:8])[CH:5]=[C:4]([N+:9]([O-])=O)[C:3]=1[CH3:12].[NH4+].[Cl-]>O.C(O)(C)C.[Fe]>[Br:1][C:2]1[C:3]([CH3:12])=[C:4]([NH2:9])[CH:5]=[C:6]([F:8])[CH:7]=1

참가 물질

6

반응물 2

HCID 25517Ammonium ChlorideHCID 27733851-Bromo-5-fluoro-2-methyl-3-nitrobenzene

생성물 1

HCID 27376413-Bromo-5-fluoro-2-methylaniline

시약·촉매·용매 3

HCID 23925Iron촉매HCID 962Water용매HCID 3776Isopropanol용매2회

반응 조건

온도
110 °C

실험 절차

To iron powder (325 mesh, 2.25 g, 40.3 mmol) in 30 ml water and 80 ml isopropanol was added commercially available 1-bromo-5-fluoro-2-methyl-3-nitro-benzene (3.04 g, 13 mmol) in 45 ml isopropanol and NH4Cl (1.46 g, 27.3 mmol). The resulting mixture was heated at 110° C. for 2 h. After evaporation of most of the isopropanol the aq solution was extracted with ethyl acetate three times. The combined organic layers were washed with water and brine, dried over MgSO4, filtered and evaporated. The crude product was used without further purification in the next step.

후처리

  1. customAfter evaporation of most of the isopropanol the aq solution
  2. extractionwas extracted with ethyl acetate three times
  3. washThe combined organic layers were washed with water and brine
  4. dry with materialdried over MgSO4
  5. filtrationfiltered
  6. customevaporated
  7. customThe crude product was used without further purification in the next step

출처 및 근거

ORD 기록
ord-e6322d2c07c0442eb0a7e6b983a5a71a
출처 데이터셋
uspto-grants-2013_02
특허 번호
US08378092B2

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