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Hydrochloric Acid → HCID 86685364, Verbindung

HRID 570701
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 570701
O1CCCC1.[CH2:6]([NH2:8])[CH3:7].CS([C:12]1[N:13]([C:24]2[CH:29]=[CH:28][C:27]([O:30][CH2:31][C:32]([F:35])([F:34])[F:33])=[CH:26][CH:25]=2)[C:14](=[O:23])[C:15]2[CH:21]=[CH:20][C:19](=[O:22])[NH:18][C:16]=2[N:17]=1)=O.Cl>O1CCCC1>[CH2:6]([NH:8][C:12]1[N:13]([C:24]2[CH:25]=[CH:26][C:27]([O:30][CH2:31][C:32]([F:35])([F:34])[F:33])=[CH:28][CH:29]=2)[C:14](=[O:23])[C:15]2[CH:21]=[CH:20][C:19](=[O:22])[NH:18][C:16]=2[N:17]=1)[CH3:7]
KomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

5

Edukt 3

HCID 313Hydrochloric AcidHCID 66726184Ethylamine tetrahydrofuranHCID 866853562-(methylsulfinyl)-3-[4-(2,2,2-trifluoroethoxy)phenyl]pyrido[2,3-d]pyrimidine-4,7(3H,8H)-dione

Produkt 1

HCID 86685364HCID 86685364, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 8028TetrahydrofuranLösungsmittel

Versuchsvorschrift

Ethylamine tetrahydrofuran solution (2M, 2 ml) was diluted with tetrahydrofuran (2 ml), 2-(methylsulfinyl)-3-[4-(2,2,2-trifluoroethoxy)phenyl]pyrido[2,3-d]pyrimidine-4,7(3H,8H)-dione (100 mg) was added thereto at room temperature, and the mixture was stirred at room temperature for 10 min. The pH of the reaction mixture was adjusted to about 7 with 0.5M hydrochloric acid (about 4 ml), and the mixture was extracted with ethyl acetate. The extract was washed with saturated brine, dried over anhydrous magnesium sulfate, and concentrated under reduced pressure. The obtained white residue was purified by silica gel column chromatography (ethyl acetate/hexane) to give the title compound (52 mg) as a white solid.

Aufarbeitung

  1. additionwas added
  2. extractionthe mixture was extracted with ethyl acetate
  3. washThe extract was washed with saturated brine
  4. dry with materialdried over anhydrous magnesium sulfate
  5. concentrationconcentrated under reduced pressure
  6. customThe obtained white residue was purified by silica gel column chromatography (ethyl acetate/hexane)

Quellen und Nachweise

ORD-Eintrag
ord-a2866b44c276486b9be88c9b4863e90a
Quelldatensatz
uspto-grants-2015_05
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US09023858B2

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