Potassium Carbonate → Hydrocarbostyril

HRID 1285440

반응식

HRID 1285440 반응식
OC([C:12]1[CH:13]=[C:14]2[C:19](=[CH:20][CH:21]=1)[NH:18][C:17](=[O:22])[CH2:16][CH2:15]2)C(N1CCNCC1)CC.BrC1C=CC(N[N+]([O-])=O)=CC=1.C(=O)([O-])[O-].[K+].[K+]>COC(C)CCO.[Cu]>[NH:18]1[C:19]2[C:14](=[CH:13][CH:12]=[CH:21][CH:20]=2)[CH2:15][CH2:16][C:17]1=[O:22]

참가 물질

6

반응물 3

HCID 11430Potassium CarbonateHCID 54478873p-BromonitroanilineHCID 570781956-(1-Hydroxy-2-piperazinylbutyl)-3,4-dihydrocarbostyril

생성물 1

HCID 64796Hydrocarbostyril

시약·촉매·용매 2

HCID 23978Copper촉매HCID 172913-Methoxy-1-butanol용매

실험 절차

5.0 Grams of 6-(1-hydroxy-2-piperazinylbutyl)-3,4-dihydrocarbostyril, 3.5 g of p-bromonitroaniline, 1.8 g of potassium carbonate and 0.2 g of copper powder were mixed in 60 ml of 3-methoxybutanol and refluxed by heating for 5 hours. The reaction mixture was filtered and the mother liquor was concentrated by distillation under a reduced pressure to dryness. The residue thus obtained was extracted with methanol-chloroform and the solvent was removed by distillation to obtain a residue. The residue was purified and separated by a preparative silica-gel thin layer chromatograph to obtain 0.21 g of 6-{1-hydroxy-2-[4-nitrophenyl)-1-piperazinyl]butyl}-3,4-dihydrocarbostyril in yellow powdery crystals.

후처리

  1. temperaturerefluxed
  2. temperatureby heating for 5 hours
  3. filtrationThe reaction mixture was filtered
  4. concentrationthe mother liquor was concentrated by distillation under a reduced pressure to dryness
  5. customThe residue thus obtained
  6. extractionwas extracted with methanol-chloroform
  7. customthe solvent was removed by distillation
  8. customto obtain a residue
  9. customThe residue was purified
  10. customseparated by a preparative silica-gel thin layer chromatograph

출처 및 근거

ORD 기록
ord-00f2d85bf9d44e13b1808a40929e5695
출처 데이터셋
uspto-grants-1986_01
특허 번호
US04567187

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