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

HRID 69407

반응식

HRID 69407 반응식
[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

참가 물질

5

반응물 3

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

생성물 1

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

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

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+).

후처리

  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

출처 및 근거

ORD 기록
ord-bfb5cb4e6bee41f1981849247ce6bbfc
출처 데이터셋
uspto-grants-2014_09
특허 번호
US08822495B2

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