StartseiteMCPWorkbenchSkills
StartseiteWorkbenchBenachrichtigungenMein Bereich
llms.txt · MCP-AnleitungDatenschutz · Nutzungsbedingungen · Supportv1.8.0
  1. Startseite
  2. /Reaktion

Hydrochloric Acid → (2S)-7-hydroxy-2-methyl-2-(trifluoromethyl)-2,3-dihydroimidazo[1,2-a]pyrimidin-5(1H)-one

HRID 633710
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 633710
Br.[CH3:2][C@@:3]1([C:9]([F:12])([F:11])[F:10])[CH2:7][NH:6][C:5]([NH2:8])=[N:4]1.C[O-].[Na+].[C:16](OCC)(=[O:23])[CH2:17][C:18](OCC)=[O:19].Cl>CO>[OH:23][C:16]1[N:8]=[C:5]2[NH:4][C@:3]([CH3:2])([C:9]([F:12])([F:10])[F:11])[CH2:7][N:6]2[C:18](=[O:19])[CH:17]=1
KomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

6

Edukt 4

HCID 313Hydrochloric AcidHCID 7761Diethyl MalonateHCID 10942334Sodium MethoxideHCID 178419517HCID 178419517, Verbindung

Produkt 1

HCID 136069601(2S)-7-hydroxy-2-methyl-2-(trifluoromethyl)-2,3-dihydroimidazo[1,2-a]pyrimidin-5(1H)-oneAusbeute 107,5 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 887
Methanol
Lösungsmittel

Versuchsvorschrift

36.90 g (148.76 mmol) of (S)-4-methyl-4-trifluoromethyl-4,5-dihydro-1H-imidazol-2-ylamine hydrobromide and 24.10 g (446 mmol) of sodium methoxide are added to a mixture of 29.50 g (216.43 mmol) of diethyl malonate in 200 mL of methanol. The resulting mixture is refluxed for 18 hours. After cooling, the mixture obtained is concentrated to dryness under vacuum. 65 mL of cold water are added to the residue obtained, to obtain a thick suspension, to which is added 25% hydrochloric acid to pH 5. The resulting suspension is stirred in an ice bath for 3 hours and then filtered. The insoluble matter obtained is rinsed with water and then dried to give 37.60 g of (S)-7-hydroxy-2-methyl-2-trifluoromethyl-2,3-dihydro-1H-imidazo[1,2-a]pyrimidin-5-one in the form of a white solid, the characteristics of which are as follows:

Aufarbeitung

  1. temperatureThe resulting mixture is refluxed for 18 hours
  2. temperatureAfter cooling
  3. customthe mixture obtained
  4. concentrationis concentrated to dryness under vacuum
  5. addition65 mL of cold water are added to the residue
  6. customobtained
  7. customto obtain a thick suspension
  8. filtrationfiltered
  9. customThe insoluble matter obtained
  10. washis rinsed with water
  11. customdried

Quellen und Nachweise

ORD-Eintrag
ord-43503273fe1b44dd9d333b8bf87d22e6
Quelldatensatz
uspto-grants-2016_04
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US09321790B2

Notizen zur Reaktion

Wird geladen…

Auf dieser SeiteKomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion