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HCID 19093752, 화합물 → HCID 19093708, 화합물

HRID 487404
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HRID 487404 반응식
C([NH:5][S:6]([C:9]1[C:10]([C:15]2[CH:20]=[CH:19][C:18]([CH2:21][N:22]3[C:31]4[C:26](=[C:27]([CH2:34][CH3:35])[N:28]=[C:29]([CH2:32][CH3:33])[CH:30]=4)[CH:25]=[CH:24][C:23]3=[O:36])=[CH:17][CH:16]=2)=[CH:11][CH:12]=[CH:13][CH:14]=1)(=[O:8])=[O:7])(C)(C)C>FC(F)(F)C(O)=O>[CH2:34]([C:27]1[N:28]=[C:29]([CH2:32][CH3:33])[CH:30]=[C:31]2[C:26]=1[CH:25]=[CH:24][C:23](=[O:36])[N:22]2[CH2:21][C:18]1[CH:19]=[CH:20][C:15]([C:10]2[C:9]([S:6]([NH2:5])(=[O:7])=[O:8])=[CH:14][CH:13]=[CH:12][CH:11]=2)=[CH:16][CH:17]=1)[CH3:35]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

3

반응물 1

HCID 19093752HCID 19093752, 화합물

생성물 1

HCID 19093708HCID 19093708, 화합물수율 77.1%

시약·촉매·용매 1

HCID 6422Trifluoroacetic acid용매

실험 절차

A solution of N-tert-butyl-4'-[(5,7-diethyl-2-oxo-1,2-dihydro-1,6-naphthyridin-1-yl)methyl]biphenyl-2-sulphonamide (200 mg) in trifluoroacetic acid (5 ml) was heated at reflux for 3 hours. Volatile material was removed by evaporation and water was added to the residue. The resultant solution was basified by the addition of solid potassium carbonate and then extracted twice with ethyl acetate. The combined extracts were washed with water, saturated sodium chloride solution and then dried (MgSO4). The solvent was removed by evaporation to give 4'-[(5,7-diethyl-2-oxo-1,2-dihydro-1,6-naphthyridin-1-yl)methyl]biphenyl-2-sulphonamide as a solid (137 mg); m.p. 199°-200° C.; NMR (d6 -DMSO): 1.18(t, 3H), 1.26(t, 3H), 2.73(q, 2H), 3.07(q, 2H), 5.54(s, 2H), 6.72(d, 1H), 7.1-7.7(m, 10H), 8.01(dd, 1H), 8.23(d, 1H); mass spectrum (+ve FAB, methanol/NBA): 448 (M+H)+ ; microanalysis, found: C, 67.0; H, 5.5; N, 9.2%; C25H25N3O3S requires: C, 67.1; H, 5.6; N, 9.4%.

후처리

  1. temperatureat reflux for 3 hours
  2. customVolatile material was removed by evaporation and water
  3. additionwas added to the residue
  4. additionThe resultant solution was basified by the addition of solid potassium carbonate
  5. extractionextracted twice with ethyl acetate
  6. washThe combined extracts were washed with water, saturated sodium chloride solution
  7. dry with materialdried (MgSO4)
  8. customThe solvent was removed by evaporation

출처 및 근거

ORD 기록
ord-ab66f4aa0ec64ea1af67dffeace2d79f
출처 데이터셋
uspto-grants-1994_03
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05294620

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