p-Fluoronitrobenzene → HCID 86681775、化合物

HRID 710599

反応式

HRID 710599 の反応式
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

参加物

6

反応物 3

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

生成物 1

HCID 86681775HCID 86681775、化合物

試薬・触媒・溶媒 2

HCID 679Dimethyl Sulfoxide溶媒HCID 8857Ethyl Acetate溶媒

反応条件

温度
100 °C

実験手順

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)+.

後処理

  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

出典と根拠

ORDレコード
ord-81b1736b12654061a6b28cc9c4969376
出典データセット
uspto-grants-2015_11
特許番号
US09181239B2

関連ノート

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