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Hydrochloric Acid → HCID 22106125、化合物

HRID 1456391
ノート
印刷プレビュー

反応式

HRID 1456391 の反応式
[CH2:1]([N:5]1[C:14]2[C:9](=[CH:10][CH:11]=[CH:12][N:13]=2)[C:8]([C:15]2[CH:20]=[CH:19][CH:18]=[C:17]([O:21][CH2:22][CH2:23][N:24](CC3C=CC=CC=3)[CH2:25][CH3:26])[CH:16]=2)=[C:7]([NH:34][C:35]([NH:37][C:38]2[C:43]([CH:44]([CH3:46])[CH3:45])=[CH:42][CH:41]=[CH:40][C:39]=2[CH:47]([CH3:49])[CH3:48])=[O:36])[C:6]1=[O:50])[CH2:2][CH2:3][CH3:4].Cl>C(O)C.[C].[Pd]>[CH2:1]([N:5]1[C:14]2[C:9](=[CH:10][CH:11]=[CH:12][N:13]=2)[C:8]([C:15]2[CH:20]=[CH:19][CH:18]=[C:17]([O:21][CH2:22][CH2:23][NH:24][CH2:25][CH3:26])[CH:16]=2)=[C:7]([NH:34][C:35]([NH:37][C:38]2[C:43]([CH:44]([CH3:46])[CH3:45])=[CH:42][CH:41]=[CH:40][C:39]=2[CH:47]([CH3:48])[CH3:49])=[O:36])[C:6]1=[O:50])[CH2:2][CH2:3][CH3:4]
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 2

HCID 313Hydrochloric AcidHCID 22105981HCID 22105981、化合物

生成物 1

HCID 22106125HCID 22106125、化合物収率 52.4%

試薬・触媒・溶媒 2

HCID 178418390HCID 178418390、化合物触媒HCID 702Ethanol溶媒

実験手順

To a solution of N-[1-butyl-4-[3-{2-(N-benzyl-N-ethylamino)ethoxy)-phenyl]-1,2-dihydro-2-oxo-1,8-naphthyridin-3-yl]-N'-(2,6-diisopropylphenyl)urea (129 mg, 0.191 mmol) in ethanol (10 ml) were added 12N aqueous hydrochloric acid solution (1 ml) and 10% palladium-carbon (210 mg), and the mixture was stirred at room temperature under hydrogen atmosphere for five hours. The mixture was filtered through a cerite pad, and the filtrate was concentrated. To the concentrated resultant was added aqueous ammonia, and the mixture was extracted with ethyl acetate. The extract was washed with water, washed with a saturated aqueous sodium chloride solution, and dried over anhydrous magnesium sulfate. The reside was concentrated under reduced pressure, and the residue was purified by thin layer chromatography (10% methanol in chloroform) to give the title compound (63 mg, 0.10 mmol).

後処理

  1. filtrationThe mixture was filtered through a cerite pad
  2. concentrationthe filtrate was concentrated
  3. concentrationTo the concentrated resultant
  4. additionwas added aqueous ammonia
  5. extractionthe mixture was extracted with ethyl acetate
  6. washThe extract was washed with water
  7. washwashed with a saturated aqueous sodium chloride solution
  8. dry with materialdried over anhydrous magnesium sulfate
  9. concentrationThe reside was concentrated under reduced pressure
  10. customthe residue was purified by thin layer chromatography (10% methanol in chloroform)

出典と根拠

ORDレコード
ord-bc9f6c2695e8477e96c5419cd58506cb
出典データセット
uspto-grants-1998_12
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05843957

反応ノート

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