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Hydrochloric Acid → HCID 54682853, 화합물

HRID 1033487
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HRID 1033487 반응식
[OH:1][C:2]1[C:11]2[C:6](=[CH:7][CH:8]=[CH:9][CH:10]=2)[NH:5][C:4](=[O:12])[C:3]=1[C:13]([OH:15])=O.[CH3:16][NH:17][C:18]1[CH:23]=[CH:22][CH:21]=[CH:20][CH:19]=1.Cl>C1(C)C=CC=CC=1>[CH3:16][N:17]([C:18]1[CH:23]=[CH:22][CH:21]=[CH:20][CH:19]=1)[C:13]([C:3]1[C:4](=[O:12])[NH:5][C:6]2[C:11]([C:2]=1[OH:1])=[CH:10][CH:9]=[CH:8][CH:7]=2)=[O:15]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 313Hydrochloric AcidHCID 7515N-MethylanilineHCID 546974994-Hydroxy-2-oxo-1,2-dihydroquinoline-3-carboxylic acid

생성물 1

HCID 54682853HCID 54682853, 화합물

시약·촉매·용매 1

HCID 1140Toluene용매

실험 절차

N,N-dicyklohexylcarbodiimide (2.2 parts) is added to a mixture consisting of 1,2-dihydro-4-hydroxy-2-oxo-quinoline-3-carboxylic acid (2.0 parts), N-metylaniline (1.1 parts) and dry toluene (25 parts) while stirring. The stirring is continued at 110° C. for 4 hrs. The reaction mixture is cooled to room temperature and the precipitate formed is filtered off. The precipitate is dissolved at pH 8.2 in 2M sodium hydroxide solution and clarified by filtration to remove the N,N-dicyklohexylurea formed. The solution is acidified with hydrochloric acid solution and the precipitate formed is filtered off. The precipitate is washed with water and methanol and dried to give N-methyl-N-phenyl-1,2-dihydro-4-hydroxy-2-oxo-quinoline-3-carboxamide, m p>300° C. (1:1).

후처리

  1. additionN,N-dicyklohexylcarbodiimide (2.2 parts) is added to a mixture
  2. customthe precipitate formed
  3. filtrationis filtered off
  4. dissolutionThe precipitate is dissolved at pH 8.2 in 2M sodium hydroxide solution
  5. filtrationclarified by filtration
  6. customto remove the N,N-dicyklohexylurea
  7. customformed
  8. customthe precipitate formed
  9. filtrationis filtered off
  10. washThe precipitate is washed with water and methanol
  11. customdried

출처 및 근거

ORD 기록
ord-259dd2f4301c4cdcb688b66ac3b753d3
출처 데이터셋
uspto-grants-1994_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05310913

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