p-Fluoronitrobenzene → HCID 86681775, 화합물

HRID 710599

반응식

HRID 710599 반응식
F[C:2]1[CH:7]=[CH:6][C:5]([N+:8]([O-:10])=[O:9])=[CH:4][CH:3]=1.[CH3:11][N:12]([CH3:20])[CH:13]1[CH2:18][CH2:17][CH:16]([NH2:19])[CH2:15][CH2:14]1.C(N(C(C)C)C(C)C)C>CS(C)=O.C(OCC)(=O)C>[CH3:11][N:12]([CH3:20])[CH:13]1[CH2:18][CH2:17][CH:16]([NH:19][C:2]2[CH:7]=[CH:6][C:5]([N+:8]([O-:10])=[O:9])=[CH:4][CH:3]=2)[CH2:15][CH2:14]1

참가 물질

6

반응물 3

HCID 9590p-FluoronitrobenzeneHCID 81531DiisopropylethylamineHCID 345823N,N-Dimethyl-1,4-cyclohexanediamine

생성물 1

HCID 86681775HCID 86681775, 화합물

시약·촉매·용매 2

HCID 679Dimethyl Sulfoxide용매HCID 8857Ethyl Acetate용매

반응 조건

온도
100 °C

실험 절차

To a solution of 1-fluoro-4-nitrobenzene (0.392 ml, 3.69 mmol) in 4 mL of dimethyl sulfoxide was added N1,N1-dimethylcyclohexane-1,4-diamine (500 mg, 3.52 mmol) and N-ethyl-N-isopropylpropan-2-amine (2.449 ml, 14.06 mmol). The reaction mixture was stirred at 100° C. for 24 hours. The mixture was poured into a separatory funnel and was diluted with 50 mL of ethyl acetate. The organic mixture was then washed with 50 mL of water followed by 50 mL of saturated aqueous brine. The organic phase was dried over sodium sulfate, filtered and concentrated. The crude material obtained was carried through the next step without purification. MS (ESI) m/z 264.1 (M+H)+.

후처리

  1. additionThe mixture was poured into a separatory funnel
  2. washThe organic mixture was then washed with 50 mL of water
  3. dry with materialThe organic phase was dried over sodium sulfate
  4. filtrationfiltered
  5. concentrationconcentrated

출처 및 근거

ORD 기록
ord-81b1736b12654061a6b28cc9c4969376
출처 데이터셋
uspto-grants-2015_11
특허 번호
US09181239B2

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