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p-Toluenesulfonic acid → 4-Ethyl-5-[(tetrahydro-2H-pyran-2-yloxy)methyl]thiophene-2-carboxaldehyde

HRID 2247736
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 2247736
[Si]([O:8][CH2:9][C:10]1[S:14][C:13]([CH2:15][OH:16])=[C:12]([CH2:17][CH3:18])[CH:11]=1)(C(C)(C)C)(C)C.[O:19]1[CH:24]=[CH:23][CH2:22][CH2:21][CH2:20]1.C1(C)C=CC(S(O)(=O)=O)=CC=1.C(=O)([O-])O.[Na+].[F-].C([N+](CCCC)(CCCC)CCCC)CCC.O1CCCC1.[Cr](O[Cr]([O-])(=O)=O)([O-])(=O)=O.[NH+]1C=CC=CC=1.[NH+]1C=CC=CC=1>ClCCl.CCOCC.O>[CH2:17]([C:12]1[CH:11]=[C:10]([CH:9]=[O:8])[S:14][C:13]=1[CH2:15][O:16][CH:20]1[CH2:21][CH2:22][CH2:23][CH2:24][O:19]1)[CH3:18]
KomponentenReaktionsbedingungenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

11

Edukt 7

HCID 6101p-Toluenesulfonic acidHCID 8028TetrahydrofuranHCID 80803,4-dihydro-2H-pyranHCID 516892Sodium BicarbonateHCID 2724130Cornforth reagentHCID 2724141Tetrabutylammonium Fluoride
HCID 68526897
[5-({[t-Butyl(dimethyl)silyl]oxy}methyl)-3-ethyl-2-thienyl]methanol

Produkt 1

HCID 866202234-Ethyl-5-[(tetrahydro-2H-pyran-2-yloxy)methyl]thiophene-2-carboxaldehydeAusbeute 78 %

Reagenzien, Katalysatoren, Lösungsmittel 3

HCID 962WaterLösungsmittel2×HCID 3283Diethyl EtherLösungsmittelHCID 6344DichloromethaneLösungsmittel

Reaktionsbedingungen

Temperatur
0 °C

Versuchsvorschrift

To a solution of [5-({[t-butyl(dimethyl)silyl]oxy}methyl)-3-ethyl-2-thienyl]methanol (1.4 g, 5.3 mmol) that was obtained in Example 22 (22a) in dichloromethane (10 ml) were added successively 3,4-dihydro-2H-pyran (0.58 ml, 6.4 mmol) and p-toluenesulfonic acid (10 mg, 0.04 mmol) at 0° C. with stirring, and the resulting mixture was stirred at room temperature for 30 minutes. After stirring, a saturated aqueous solution of sodium hydrogencarbonate (5 ml) was added to the reaction mixture to quench the reaction, and the resulting mixture was poured into water (20 ml) and extracted with ether. The extract was washed with a saturated aqueous solution of sodium chloride and dried over magnesium sulfate. After filtration, the filtrate was evaporated in vacuo. Subsequently, to a solution of the residue obtained in tetrahydrofuran (5 ml) was added a 1.0 M solution of tetrabutylammonium fluoride in tetrahydrofuran (6.4 ml, 6.4 mmol) with stirring, and the resulting mixture was stirred at room temperature for 30 minutes. After stirring, the reaction mixture was poured into water (20 ml) and extracted with ether. The extract was washed with a saturated aqueous solution of sodium chloride and dried over magnesium sulfate. After filtration, the filtrate was evaporated in vacuo. Subsequently, to a solution of the residue obtained in dichloromethane (30 ml) was added molecular sieves 4A (10g), and after cooling to 0° C., pyridinium dichromate (3.3 g, 8.7 mmol) was furthermore added to the resulting mixture with stirring, and the resulting mixture was stirred at room temperature for 2 hours. After stirring, ether (150 ml) was added to the reaction mixture with stirring, and insoluble materials were removed by filtration with silica gel. The filtrate was evaporated in vacuo, and the crude product of the title compound thus obtained was purified by chromatography on a silica gel column using a mixed solvent of ethyl acetate and hexane (0:10 to 2:8) as the eluent to afford the title compound (0.97 g) in a yield of 78% as a colourless oily product.

Aufarbeitung

  1. stirringthe resulting mixture was stirred at room temperature for 30 minutes
  2. stirringAfter stirring
  3. customto quench
  4. customthe reaction
  5. extractionextracted with ether
  6. washThe extract was washed with a saturated aqueous solution of sodium chloride
  7. dry with materialdried over magnesium sulfate
  8. filtrationAfter filtration
  9. customthe filtrate was evaporated in vacuo
  10. customSubsequently, to a solution of the residue obtained in tetrahydrofuran (5 ml)
  11. stirringwith stirring
  12. stirringthe resulting mixture was stirred at room temperature for 30 minutes
  13. stirringAfter stirring
  14. extractionextracted with ether
  15. washThe extract was washed with a saturated aqueous solution of sodium chloride
  16. dry with materialdried over magnesium sulfate
  17. filtrationAfter filtration
  18. customthe filtrate was evaporated in vacuo
  19. customSubsequently, to a solution of the residue obtained in dichloromethane (30 ml)
  20. stirringwith stirring
  21. stirringthe resulting mixture was stirred at room temperature for 2 hours
  22. stirringAfter stirring
  23. stirringwith stirring
  24. custominsoluble materials were removed by filtration with silica gel
  25. customThe filtrate was evaporated in vacuo

Quellen und Nachweise

ORD-Eintrag
ord-5ed2fab7a0a24c7ba54fd066bca2dc18
Quelldatensatz
uspto-grants-2010_03
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US07687491B2

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