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

Potassium Iodide → [4-amino-1-(tetrahydro-2H-pyran-4-ylmethyl)-1H-imidazo[4,5-c]quinolin-2-yl]methanol

HRID 81928
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 81928
[C:1]([O-:4])(=O)[CH3:2].[K+].[I-].[K+].ClCC1[N:11]([CH2:24][CH:25]2[CH2:30][CH2:29][O:28][CH2:27][CH2:26]2)[C:12]2[C:21]3[CH:20]=[CH:19][CH:18]=[CH:17][C:16]=3[N:15]=[C:14]([NH2:22])[C:13]=2[N:23]=1.O.[OH-].[Li+]>O>[NH2:22][C:14]1[C:13]2[N:23]=[C:2]([CH2:1][OH:4])[N:11]([CH2:24][CH:25]3[CH2:30][CH2:29][O:28][CH2:27][CH2:26]3)[C:12]=2[C:21]2[CH:20]=[CH:19][CH:18]=[CH:17][C:16]=2[N:15]=1
KomponentenReaktionsbedingungenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

6

Edukt 4

HCID 4875Potassium IodideHCID 168937Lithium hydroxide, monohydrateHCID 517044Potassium AcetateHCID 67262961HCID 67262961, Verbindung

Produkt 1

HCID 57555858[4-amino-1-(tetrahydro-2H-pyran-4-ylmethyl)-1H-imidazo[4,5-c]quinolin-2-yl]methanolAusbeute 38,6 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 962
Water
Lösungsmittel

Reaktionsbedingungen

Temperatur
50 °C

Versuchsvorschrift

Potassium acetate (0.41 g, 4.16 mmol) and potassium iodide (0.28 g, 1.66 mmol) were added to a stirring solution of 2-(chloromethyl)-1-(tetrahydro-2H-pyran-4-ylmethyl)-1H-imidazo[4,5-c]quinolin-4-amine (0.55 g, 1.66 mmol) and the resulting suspension was heated to 50° C. After 17 hours, the suspension was cooled to ambient temperature and concentrated under reduced pressure. The residue was suspended in methanol (10 mL) and water (5 mL) and lithium hydroxide monohydrate (0.35 g, 8.31 mmol) was added in one portion. The resulting solution was stirred at ambient temperature 18 hours and concentrated under reduced pressure. The residue was diluted with water (20 mL) and neutralized with hydrochloric acid (6 N in water). The aqueous layer was extracted with dichloromethane (2×50 mL) and ethyl acetate (50 mL). The combined organic fractions were concentrated to a yellow solid which was crystallized from acetonitrile. The crystals were isolated by filtration and dried in a vacuum oven at 65° C. to provide 0.20 g of [4-amino-1-(tetrahydro-2H-pyran-4-ylmethyl)-1H-imidazo[4,5-c]quinolin-2-yl]methanol as an off-white solid, mp 239-241° C.

Aufarbeitung

  1. temperaturethe suspension was cooled to ambient temperature
  2. concentrationconcentrated under reduced pressure
  3. concentrationconcentrated under reduced pressure
  4. additionThe residue was diluted with water (20 mL)
  5. extractionThe aqueous layer was extracted with dichloromethane (2×50 mL) and ethyl acetate (50 mL)
  6. concentrationThe combined organic fractions were concentrated to a yellow solid which
  7. customwas crystallized from acetonitrile
  8. customThe crystals were isolated by filtration
  9. customdried in a vacuum oven at 65° C.

Quellen und Nachweise

ORD-Eintrag
ord-8a3a8fe19fec4f7bbc15a8aa713776c0
Quelldatensatz
uspto-grants-2014_09
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US08846710B2

Notizen zur Reaktion

Wird geladen…

Auf dieser SeiteKomponentenReaktionsbedingungenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion