Potassium Carbonate → [1-(2-Chloro-4-nitrophenyl)pyrrolidin-3-yl]dimethylamine

HRID 69407

反応式

HRID 69407 の反応式
[Cl:1][C:2]1[CH:7]=[C:6]([N+:8]([O-:10])=[O:9])[CH:5]=[CH:4][C:3]=1F.[CH3:12][N:13]([CH3:19])[CH:14]1[CH2:18][CH2:17][NH:16][CH2:15]1.C(=O)([O-])[O-].[K+].[K+]>CN(C=O)C>[Cl:1][C:2]1[CH:7]=[C:6]([N+:8]([O-:10])=[O:9])[CH:5]=[CH:4][C:3]=1[N:16]1[CH2:17][CH2:18][CH:14]([N:13]([CH3:19])[CH3:12])[CH2:15]1

参加物

5

反応物 3

HCID 11430Potassium CarbonateHCID 676882-Chloro-1-fluoro-4-nitrobenzeneHCID 27585193-(Dimethylamino)pyrrolidine

生成物 1

HCID 53440459[1-(2-Chloro-4-nitrophenyl)pyrrolidin-3-yl]dimethylamine

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

A mixture of 2-chloro-1-fluoro-4-nitrobenzene (4.79 g), dimethylpyrrolidin-3-ylamine (2.60 g), potassium carbonate (3.82 g) and DMF (35 mL) was stirred at room temperature for 4 hours. The reaction mixture was partitioned between water and ethyl acetate. The organic phase was extracted with hydrochloric acid (2 M), and the extract was basified with sodium hydroxide solution (2M). Extraction with ethyl acetate afforded an organic phase which was dried and concentrated. The product with the molecular weight of 269.73 (C12H16ClN3O2) was obtained in this way; MS (ESI): 270 (M+H+).

後処理

  1. customThe reaction mixture was partitioned between water and ethyl acetate
  2. extractionThe organic phase was extracted with hydrochloric acid (2 M)
  3. extractionExtraction with ethyl acetate
  4. customafforded an organic phase which
  5. customwas dried
  6. concentrationconcentrated
  7. customThe product with the molecular weight of 269.73 (C12H16ClN3O2) was obtained in this way

出典と根拠

ORDレコード
ord-bfb5cb4e6bee41f1981849247ce6bbfc
出典データセット
uspto-grants-2014_09
特許番号
US08822495B2

関連ノート

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