Methanol → HCID 178493687, Verbindung

HRID 627617Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 627617
Cl[C:2]1[CH:11]=[N:10][C:9]2[C:8](=[O:12])[N:7]=[CH:6][NH:5][C:4]=2[CH:3]=1.[CH3:13][O-:14].[Na+].CO.[Cl-].[NH4+]>>[CH3:13][O:14][C:2]1[CH:11]=[N:10][C:9]2[C:8](=[O:12])[N:7]=[CH:6][NH:5][C:4]=2[CH:3]=1

Komponenten

5

Edukt 4

HCID 887MethanolHCID 25517Ammonium ChlorideHCID 10942334Sodium Methoxide2×HCID 1785182197-chloro-1H-pyrido[3,2-d]pyrimidin-4-one

Produkt 1

HCID 178493687HCID 178493687, Verbindung

Versuchsvorschrift

A microwave vial was charged with 7-chloropyrido[3,2-d]pyrimidin-4(1H)-one (110 mg, 0.606 mmol), a 0.5 M solution of sodium methoxide in methanol (3.65 mL, 1.817 mmol) and sodium methoxide (327 mg, 6.06 mmol). The vial was capped and irradiated in a microwave reactor at 145° C. for 30 minutes. The reaction was neutralized with saturated aqueous ammonium chloride (3 mL), concentrated, and diluted with cold water. The resulting precipitate was collected by vacuum filtration and dried in vacuo to provide the title compound (107 mg, 0.604 mmol) as pink solid. 1H NMR (400 MHz, DMSO-d6) δ ppm 3.95 (s, 3H) 7.49 (d, J=2.74 Hz, 1H) 8.11 (s, 1H) 8.47 (d, J=2.74 Hz, 1H). LC/MS (ESI+) m/z=178 (M+H).

Aufarbeitung

  1. customThe vial was capped
  2. customirradiated in a microwave reactor at 145° C. for 30 minutes
  3. concentrationconcentrated
  4. additiondiluted with cold water
  5. filtrationThe resulting precipitate was collected by vacuum filtration
  6. customdried in vacuo

Quellen und Nachweise

ORD-Eintrag
ord-19bfcbdf23124e43a61d93adc825c270
Quelldatensatz
uspto-grants-2016_04
Patentnummer
US09309263B2

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