Potassium Carbonate → HCID 69161998、化合物

HRID 409692

反応式

HRID 409692 の反応式
[CH2:1]([N:3]1[CH2:8][CH2:7][NH:6][CH2:5][CH2:4]1)[CH3:2].[Cl:9][C:10]1[CH:15]=[C:14](F)[CH:13]=[CH:12][C:11]=1[N+:17]([O-:19])=[O:18].C(=O)([O-])[O-].[K+].[K+]>CN(C=O)C.O>[Cl:9][C:10]1[CH:15]=[C:14]([N:6]2[CH2:7][CH2:8][N:3]([CH2:1][CH3:2])[CH2:4][CH2:5]2)[CH:13]=[CH:12][C:11]=1[N+:17]([O-:19])=[O:18]

参加物

6

反応物 3

HCID 11430Potassium CarbonateHCID 750172-Chloro-4-fluoro-1-nitrobenzeneHCID 791961-Ethylpiperazine

生成物 1

HCID 69161998HCID 69161998、化合物収率 72.6%

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 6228Dimethylformamide溶媒

反応条件

温度
100 °C

実験手順

N-Ethylpiperazine (4.3 mL, 34.3 mmol, 1.2 equiv) is added to a mixture of 2-chloro-4-fluoronitrobenzene (5 g, 28.6 mmol) and potassium carbonate (7.9 g, 57.1 mmol, 2 equiv) in DMF (50 mL). The reaction mixture is stirred at 100° C. for 6 h, allowed to cool to RT, diluted with H2O and extracted with EtOAc. The organic phase is washed with brine, dried (Na2SO4), filtered and concentrated. The residue is purified by trituration in diethyl ether to provide 5.6 g of the title compound as a yellow solid: ES-MS: 270.0 [MH]+; tR=2.90 min (system 1).

後処理

  1. temperatureto cool to RT
  2. extractionextracted with EtOAc
  3. washThe organic phase is washed with brine
  4. dry with materialdried (Na2SO4)
  5. filtrationfiltered
  6. concentrationconcentrated
  7. customThe residue is purified by trituration in diethyl ether

出典と根拠

ORDレコード
ord-3e7fc2a34c1e49d3b9f834f4b314766b
出典データセット
uspto-grants-2014_06
特許番号
US08759517B2

関連ノート

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