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Hydrochloric Acid → 3,5-dimethyl-4-hydroxy-6-(5-(5-pyrimidinylmethoxy)benzofuran-2-yl)-2H-pyran-2-one

HRID 1357213
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Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 1357213
C(P(CCCC)CCCC)CCC.CN(C(/N=N/C(N(C)C)=O)=O)C.C([O:29][C:30]1[C:35]([CH3:36])=[C:34]([C:37]2[O:38][C:39]3[CH:45]=[CH:44][C:43](O)=[CH:42][C:40]=3[CH:41]=2)[O:33][C:32](=[O:47])[C:31]=1[CH3:48])(=O)C.[OH:49][CH2:50][C:51]1[CH:52]=[N:53][CH:54]=[N:55][CH:56]=1.[OH-].[Li+].Cl>C1COCC1.C(Cl)Cl.CCOC(C)=O>[CH3:48][C:31]1[C:32](=[O:47])[O:33][C:34]([C:37]2[O:38][C:39]3[CH:45]=[CH:44][C:43]([O:49][CH2:50][C:51]4[CH:52]=[N:53][CH:54]=[N:55][CH:56]=4)=[CH:42][C:40]=3[CH:41]=2)=[C:35]([CH3:36])[C:30]=1[OH:29]
KomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

10

Edukt 6

HCID 313Hydrochloric AcidHCID 3939Lithium HydroxideHCID 13831TributylphosphineHCID 5353800DiamideHCID 15466386(Pyrimidin-5-yl)methanolHCID 185058904-acetyloxy-3,5-dimethyl-6-(5-hydroxybenzofuran-2-yl)-2H-pyran-2-one

Produkt 1

HCID 54738107
3,5-dimethyl-4-hydroxy-6-(5-(5-pyrimidinylmethoxy)benzofuran-2-yl)-2H-pyran-2-one

Reagenzien, Katalysatoren, Lösungsmittel 3

HCID 6344DichloromethaneLösungsmittelHCID 8028TetrahydrofuranLösungsmittel2×HCID 8857Ethyl AcetateLösungsmittel

Versuchsvorschrift

A solution of tributylphosphine in 2 N THF (0.94 ml) and a solution of TMAD (323 mg) in CH2Cl2 (3 ml) were added dropwise to a solution of 4-acetyloxy-3,5-dimethyl-6-(5-hydroxybenzofuran-2-yl)-2H-pyran-2-one (118 mg) and 5-hydroxymethylpyrimidine (202 mg) in THF (30 ml) at 0° C., and the mixture was stirred at room temperature overnight. The reaction solution was cooled on ice, a 1 N lithium hydroxide aqueous solution (5 ml) was added and the mixture was stirred at room temperature for one hour, after which the reaction solution was again cooled on ice, a 1 N hydrochloric acid aqueous solution (5 ml) and AcOEt were added, the organic layer and aqueous layer were separated, and the aqueous layer was further extracted with AcOEt. The organic layers were combined and dried with MgSO4, and then filtered and concentrated. The residue was purified by silica gel column chromatography (AcOEt/MeOH=10/1) to obtain 3,5-dimethyl-4-hydroxy-6-(5-(5-pyrimidinylmethoxy)benzofuran-2-yl)-2H-pyran-2-one.

Aufarbeitung

  1. temperatureThe reaction solution was cooled on ice
  2. stirringthe mixture was stirred at room temperature for one hour
  3. temperatureafter which the reaction solution was again cooled on ice
  4. customthe organic layer and aqueous layer were separated
  5. extractionthe aqueous layer was further extracted with AcOEt
  6. dry with materialdried with MgSO4
  7. filtrationfiltered
  8. concentrationconcentrated
  9. customThe residue was purified by silica gel column chromatography (AcOEt/MeOH=10/1)

Quellen und Nachweise

ORD-Eintrag
ord-81a702c01d49401bb595755b1d9d5695
Quelldatensatz
uspto-grants-2003_07
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US06589984B1

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