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Trimethylsilyl triflate → 4-(4-ethylphenylmethyl)-1-(2,3,4,6-tetra-O-acetyl-beta-D-glucopyranosyl) pyrazole

HRID 220999
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 220999
[CH2:1]([C:3]1[CH:8]=[CH:7][C:6]([CH2:9][C:10]2[CH:11]=[N:12][NH:13][CH:14]=2)=[CH:5][CH:4]=1)[CH3:2].C/C(/O[Si](C)(C)C)=N\[Si](C)(C)C.C(O[C@@H:31]1[O:48][C@H:47]([CH2:49][O:50][C:51](=[O:53])[CH3:52])[C@@H:42]([O:43][C:44](=[O:46])[CH3:45])[C@H:37]([O:38][C:39](=[O:41])[CH3:40])[C@H:32]1[O:33][C:34](=[O:36])[CH3:35])(=O)C.FC(F)(F)S(O[Si](C)(C)C)(=O)=O>C(#N)C.ClC(Cl)C>[CH2:1]([C:3]1[CH:8]=[CH:7][C:6]([CH2:9][C:10]2[CH:11]=[N:12][N:13]([C@@H:31]3[O:48][C@H:47]([CH2:49][O:50][C:51](=[O:53])[CH3:52])[C@@H:42]([O:43][C:44](=[O:46])[CH3:45])[C@H:37]([O:38][C:39](=[O:41])[CH3:40])[C@H:32]3[O:33][C:34](=[O:36])[CH3:35])[CH:14]=2)=[CH:5][CH:4]=1)[CH3:2]
KomponentenReaktionsbedingungenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

7

Edukt 4

HCID 65367Trimethylsilyl triflateHCID 2724702beta-D-Glucose pentaacetateHCID 6913588N,O-bis(trimethylsilyl)acetamideHCID 582426374-(4-Ethylphenylmethyl)pyrazole

Produkt 1

HCID 666076354-(4-ethylphenylmethyl)-1-(2,3,4,6-tetra-O-acetyl-beta-D-glucopyranosyl) pyrazoleAusbeute 44,4 %

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 6342AcetonitrileLösungsmittelHCID 63651,1-DichloroethaneLösungsmittel

Reaktionsbedingungen

Temperatur
60 °C

Versuchsvorschrift

To a solution of 4-(4-ethylphenylmethyl)pyrazole 36 (495 mg) in acetonitrile (2.0 ml) was added N,O-bis(trimethylsilyl)acetamide (1.05 ml), and the mixture was stirred under heating at 60° C. for 2.5 hours under argon atmosphere. The reaction mixture was cooled to room temperature, and the solvent was evaporated under reduced pressure to give crude 4-(4-ethylphenylmethyl)-1-trimethylsilylpyrazole 37, which was used in the subsequent reaction without further purification. (2) The above N-silyl compound 37 was dissolved in dichloroethane (7.0 ml), and added thereto were molecular sieve 4A powder (500 mg), 1,2,3,4,6-penta-O-acetyl-β-D-glucopyranose 38 (1.04 g) and trimethylsilyl trifluoromethanesulfonate (0.51 ml). The mixture was stirred under heating at heating at 80° C. for 3 hours under argon atmosphere. The reaction mixture was cooled to room temperature, and insoluble materials were filtered off. Subsequently, the filtrate was poured into a saturated aqueous sodium hydrogen carbonate solution. The mixture was extracted twice with dichloromethane, and dried over sodium sulfate. The solvent was evaporated under reduced pressure, and the residue was purified by silica gel column chromatography (hexane:ethyl acetate=80:20-50:50) to give 4-(4-ethylphenylmethyl)-1-(2,3,4,6-tetra-O-acetyl-β-D-glucopyranosyl)pyrazole 39 (610 mg) as a colorless semisolid. APCI-Mass m/Z 517 (M+H). (3) From the above tetraacetate compound 39, the desired 4-(4-ethylphenylmethyl)-1-(β-D-glucopyranosyl)pyrazole 40 was prepared in a manner similar to Example 106-(3) as colorless oil. APCI-Mass m/Z 349 (M+H).

Aufarbeitung

  1. temperatureThe reaction mixture was cooled to room temperature
  2. customthe solvent was evaporated under reduced pressure
  3. customto give crude 4-(4-ethylphenylmethyl)-1-trimethylsilylpyrazole 37, which
  4. customwas used in the subsequent reaction without further purification
  5. additionadded
  6. stirringThe mixture was stirred
  7. temperatureunder heating
  8. temperatureat heating at 80° C. for 3 hours under argon atmosphere
  9. temperatureThe reaction mixture was cooled to room temperature
  10. filtrationinsoluble materials were filtered off
  11. additionSubsequently, the filtrate was poured into a saturated aqueous sodium hydrogen carbonate solution
  12. extractionThe mixture was extracted twice with dichloromethane
  13. dry with materialdried over sodium sulfate
  14. customThe solvent was evaporated under reduced pressure
  15. customthe residue was purified by silica gel column chromatography (hexane:ethyl acetate=80:20-50:50)

Quellen und Nachweise

ORD-Eintrag
ord-548c4724a7ba40cdb37aee8df9960643
Quelldatensatz
uspto-grants-2012_06
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US08202984B2

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