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Cesium carbonate → (1Z)-1-[3-(5-methyl-2-propan-2-ylphenyl)-4-oxo-1,3-thiazolidin-2-ylidene]-3-[1-[4-[1-[4-(trifluoromethoxy)phenyl]-1,2,4-triazol-3-yl]phenyl]propan-2-yl]urea

HRID 573844
ノート
印刷プレビュー

反応式

HRID 573844 の反応式
[N:1]([CH:4]([CH3:28])[CH2:5][C:6]1[CH:11]=[CH:10][C:9]([C:12]2[N:16]=[CH:15][N:14]([C:17]3[CH:22]=[CH:21][C:20]([O:23][C:24]([F:27])([F:26])[F:25])=[CH:19][CH:18]=3)[N:13]=2)=[CH:8][CH:7]=1)=[C:2]=[O:3].[N-]=C=O.[CH:32]([C:35]1[CH:40]=[CH:39][C:38]([CH3:41])=[CH:37][C:36]=1[NH:42][C:43]([NH2:45])=[S:44])([CH3:34])[CH3:33].C(=O)([O-])[O-].[Cs+].[Cs+].[C:52]([O-])(=[O:54])[CH3:53].[Na+].BrCC(OC)=O>C(#N)C.C(O)C.C(OCC)(=O)C>[CH:32]([C:35]1[CH:40]=[CH:39][C:38]([CH3:41])=[CH:37][C:36]=1[N:42]1[C:52](=[O:54])[CH2:53][S:44]/[C:43]/1=[N:45]\[C:2]([NH:1][CH:4]([CH3:28])[CH2:5][C:6]1[CH:11]=[CH:10][C:9]([C:12]2[N:16]=[CH:15][N:14]([C:17]3[CH:22]=[CH:21][C:20]([O:23][C:24]([F:26])([F:25])[F:27])=[CH:19][CH:18]=3)[N:13]=2)=[CH:8][CH:7]=1)=[O:3])([CH3:34])[CH3:33]
参加物実験手順後処理出典と根拠反応ノート

参加物

10

反応物 6

HCID 10796Cesium carbonateHCID 60984Methyl bromoacetateHCID 105034IsocyanateHCID 517045Sodium AcetateHCID 893731681-(2-Isopropyl-5-methylphenyl)thioureaHCID 904040983-(4-(2-isocyanatopropyl)phenyl)-1-(4-(trifluoromethoxy)phenyl)-1H-1,2,4-triazole

生成物 1

HCID 90404514
(1Z)-1-[3-(5-methyl-2-propan-2-ylphenyl)-4-oxo-1,3-thiazolidin-2-ylidene]-3-[1-[4-[1-[4-(trifluoromethoxy)phenyl]-1,2,4-triazol-3-yl]phenyl]propan-2-yl]urea
収率 20.7%

試薬・触媒・溶媒 3

HCID 702Ethanol溶媒HCID 6342Acetonitrile溶媒HCID 8857Ethyl Acetate溶媒

実験手順

3-(4-(2-Isocyanatopropyl)phenyl)-1-(4-(trifluoromethoxy)phenyl)-1H-1,2,4-triazole (C39) (0.17 g, 0.41 mmol) in acetonitrile (2 mL) was heated at 80° C. for 2 hours to ensure complete conversion to the isocyanate. The reaction was cooled and 1-(2-isopropyl-5-methylphenyl)thiourea (0.095 g, 0.46 mmol) and cesium carbonate (0.20 g, 0.60 mmol) were added. The reaction was stirred at room temperature for 3 days. The reaction was diluted with ethanol (2.5 mL) and sodium acetate (0.064 g, 0.78 mmol) and methyl 2-bromoacetate (0.05 mL, 0.53 mmol) were added. The reaction was heated at 65° C. for 2.5 hours. The reaction mixture was diluted with ethyl acetate and washed with water. The aqueous layer was extracted an additional time with ethyl acetate. The combined organic layers were dried over anhydrous sodium sulfate, filtered, and concentrated. The crude material was loaded onto a Celite® cartridge and purified by flash column chromatography using 0-100% ethyl acetate/B, where B=1:1 dichloromethane/hexanes, as eluent to afford the title compound as an off-white solid (0.054 g, 20%).

後処理

  1. temperatureThe reaction was cooled
  2. additionwere added
  3. temperatureThe reaction was heated at 65° C. for 2.5 hours
  4. washwashed with water
  5. extractionThe aqueous layer was extracted an additional time with ethyl acetate
  6. dry with materialThe combined organic layers were dried over anhydrous sodium sulfate
  7. filtrationfiltered
  8. concentrationconcentrated
  9. custompurified by flash column chromatography

出典と根拠

ORDレコード
ord-62931b11946d46d7bd220da26c2c2ebd
出典データセット
uspto-grants-2015_05
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09029560B2

反応ノート

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