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Isopropanol → 1-Benzenesulphonyl-5-methoxy-3-[(2-pyrrolidin-1-yl)ethyl]-1H-indole Hydrogen Oxalate

HRID 635382
ノート
印刷プレビュー

反応式

HRID 635382 の反応式
[C:1]1([S:7]([N:10]2[C:18]3[C:13](=[CH:14][C:15]([O:19][CH3:20])=[CH:16][CH:17]=3)[C:12]([CH2:21][CH2:22][O:23]S(C3C=CC=CC=3)(=O)=O)=[CH:11]2)(=[O:9])=[O:8])[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.[C:33](=[O:36])([O-:35])[O-].[K+].[K+].[NH:39]1[CH2:43][CH2:42][CH2:41][CH2:40]1.CC([OH:47])C>>[C:22]([OH:23])(=[O:47])[C:33]([OH:35])=[O:36].[C:1]1([S:7]([N:10]2[C:18]3[C:13](=[CH:14][C:15]([O:19][CH3:20])=[CH:16][CH:17]=3)[C:12]([CH2:21][CH2:22][N:39]3[CH2:43][CH2:42][CH2:41][CH2:40]3)=[CH:11]2)(=[O:9])=[O:8])[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 4

HCID 3776Isopropanol2 回HCID 11430Potassium CarbonateHCID 31268PyrrolidineHCID 11762460benzenesulphonic acid 2-(1-benzenesulphonyl-5-methoxy-1H-indol-3-yl)ethyl ester

生成物 1

HCID 212585631-Benzenesulphonyl-5-methoxy-3-[(2-pyrrolidin-1-yl)ethyl]-1H-indole Hydrogen Oxalate収率 65%

実験手順

To a stirred solution of benzenesulphonic acid 2-(1-benzenesulphonyl-5-methoxy-1H-indol-3-yl)ethyl ester (0.191 g, 0.405 mmol) in anhydrous 2-propanol (10 ml) under nitrogen was added anhydrous potassium carbonate (0.112 g, 0.810 mmol), then a solution of pyrrolidine (0.17 ml, 2.03 mmol) in anhydrous 2-propanol (3 ml). The mixture was heated at reflux for 4 h, and the solvents were then removed in vacuo. The residue was partitioned between dichloromethane and water, and the aqueous layer was extracted further with dichloromethane. The combined organic extracts were washed with brine (2×25 ml), dried (Na2SO4), and evaporated in vacuo. The residue was purified by flash chromatography (silica gel, CH2Cl2—MeOH—NH3; 95:5:0.5) to give 0.102 g (65%) of the title compound free base. The oxalate salt was prepared in EtOH-Et2O as a white solid; mp 217°-220° C.; δH (360 MHz, d6-DMSO) 1.94 (4H, s), 3.03 (2H, m), 3.27 (4H, s), 3.40 (2H, m), 3.79 (3H, s), 6.98 (1H, dd, J=9.0, 2.3 Hz), 7.17 (1H, d, J=2.3 Hz), 7.58 (2H, t, J=8.0 Hz), 7.69 (2H, m), 7.82 (1H, d, J=9.0 Hz), 7.92 (2H, d, J=7.9 Hz); m/z (ES+) 385 (MH30 ). Found: C, 57.83; H, 5.31; N, 5.87. C21H24N2O3S.C2H2O4 requires C, 58.22; H, 5.52; N, 5.90%.

後処理

  1. temperatureThe mixture was heated
  2. temperatureat reflux for 4 h
  3. customthe solvents were then removed in vacuo
  4. customThe residue was partitioned between dichloromethane and water
  5. extractionthe aqueous layer was extracted further with dichloromethane
  6. washThe combined organic extracts were washed with brine (2×25 ml)
  7. dry with materialdried (Na2SO4)
  8. customevaporated in vacuo
  9. customThe residue was purified by flash chromatography (silica gel, CH2Cl2—MeOH—NH3; 95:5:0.5)

出典と根拠

ORDレコード
ord-811ee4f4c3e6424b99addb7617f0a8f3
出典データセット
uspto-grants-2001_02
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06187805B1

反応ノート

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