5-fluoro-N-methyl-2-nitroaniline → 5-Fluoro-N1-methylbenzene-1,2-diamine

HRID 1048937노트

반응식

HRID 1048937 반응식
[F:1][C:2]1[CH:3]=[CH:4][C:5]([N+:10]([O-])=O)=[C:6]([CH:9]=1)[NH:7][CH3:8]>[Pd].CO>[F:1][C:2]1[CH:9]=[C:6]([NH:7][CH3:8])[C:5]([NH2:10])=[CH:4][CH:3]=1

참가 물질

4

반응물 1

HCID 229057745-fluoro-N-methyl-2-nitroaniline

생성물 1

HCID 184572835-Fluoro-N1-methylbenzene-1,2-diamine

시약·촉매·용매 2

HCID 23938Palladium촉매HCID 887Methanol용매

실험 절차

To the title compound from Example 1 Step A (0.267 g, 1.57 mmol) were added palladium on carbon (0.027 g) and methanol (7.85 mL). The resulting mixture was stirred under an atmosphere of hydrogen at room temperature overnight. The mixture was then filtered through CELITE® using dichloromethane, and the filtrate was concentrated. Purification by flash chromatography (50% ethyl acetate in hexanes, then 100% ethyl acetate) provided the title compound: 1H NMR (500 MHz, CDCl3) δ 6.61 (dd, J=8.2, 5.6 Hz, 1 H), 6.36-6.30 (m, 2 H), 3.22 (br s, 3 H), 2.84 (s, 3 H).

후처리

  1. filtrationThe mixture was then filtered through CELITE®
  2. concentrationthe filtrate was concentrated
  3. customPurification by flash chromatography (50% ethyl acetate in hexanes

출처 및 근거

ORD 기록
ord-33b884d3682748a2a1cef0f56413be90
출처 데이터셋
uspto-grants-2016_07
특허 번호
US09382226B2

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