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Hydrochloric Acid → HCID 86640673, Verbindung

HRID 1645231
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 1645231
[F:1][C:2]([F:6])([F:5])[CH2:3][OH:4].[H-].[Na+].Br[CH2:10][C:11]1[CH:16]=[C:15]([C:17]2[C:22]([Cl:23])=[CH:21][C:20]([C:24]([F:27])([F:26])[F:25])=[CH:19][N:18]=2)[N:14]2[N:28]=[CH:29][N:30]=[C:13]2[N:12]=1.Cl>O1CCCC1>[Cl:23][C:22]1[C:17]([C:15]2[N:14]3[N:28]=[CH:29][N:30]=[C:13]3[N:12]=[C:11]([CH2:10][O:4][CH2:3][C:2]([F:6])([F:5])[F:1])[CH:16]=2)=[N:18][CH:19]=[C:20]([C:24]([F:26])([F:25])[F:27])[CH:21]=1
KomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

6

Edukt 4

HCID 313Hydrochloric AcidHCID 64092,2,2-TrifluoroethanolHCID 24758Sodium hydrideHCID 66775659HCID 66775659, Verbindung

Produkt 1

HCID 86640673HCID 86640673, VerbindungAusbeute 30,8 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 8028
Tetrahydrofuran
Lösungsmittel

Versuchsvorschrift

230 mg of 2,2,2-trifluoroethanol was added to a tetrahydrofuran (dehydrated) 8 mL solution of 33 mg of 60% sodium hydride, followed by stirring for 5 minutes, and 300 mg of 5-bromomethyl-7-(3-chloro-5-(trifluoromethyl)pyridin-2-yl)-[1,2,4]triazolo[1,5-a]pyrimidine was added at room temperature, followed by stirring for 5 minutes. After completion of the reaction, 1N hydrochloric acid was added to make it acidic, followed by extraction with ethyl acetate, the organic layer was dried over anhydrous sodium sulfate, and the solvent was distilled off under reduced pressure. The residue was purified by silica gel column chromatography (eluent: n-hexane/ethyl acetate=1/1) to obtain 97 mg of the desired product.

Aufarbeitung

  1. stirringby stirring for 5 minutes
  2. additionwas added
  3. extractionfollowed by extraction with ethyl acetate
  4. dry with materialthe organic layer was dried over anhydrous sodium sulfate
  5. distillationthe solvent was distilled off under reduced pressure
  6. customThe residue was purified by silica gel column chromatography (eluent: n-hexane/ethyl acetate=1/1)

Quellen und Nachweise

ORD-Eintrag
ord-3a39aaf838ea424a88e46147c48e0f6a
Quelldatensatz
uspto-grants-2012_02
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US08124760B2

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