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HCID 19093752、化合物 → HCID 19093708、化合物

HRID 487404
ノート
印刷プレビュー

反応式

HRID 487404 の反応式
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]
参加物実験手順後処理出典と根拠反応ノート

参加物

3

反応物 1

HCID 19093752HCID 19093752、化合物

生成物 1

HCID 19093708HCID 19093708、化合物収率 77.1%

試薬・触媒・溶媒 1

HCID 6422Trifluoroacetic acid溶媒

実験手順

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%.

後処理

  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

出典と根拠

ORDレコード
ord-ab66f4aa0ec64ea1af67dffeace2d79f
出典データセット
uspto-grants-1994_03
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05294620

反応ノート

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