Potassium Carbonate → 6-(6-chloropyrimidin-4-yloxy)-2-(methoxymethyl)-4-methyl-1H-benzo[d]imidazole

HRID 1846466Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1846466
[CH3:1][O:2][CH2:3][C:4]1[NH:8][C:7]2[CH:9]=[C:10]([OH:14])[CH:11]=[C:12]([CH3:13])[C:6]=2[N:5]=1.[Cl:15][C:16]1[CH:21]=[C:20](Cl)[N:19]=[CH:18][N:17]=1.C(=O)([O-])[O-].[K+].[K+]>CN(C=O)C>[Cl:15][C:16]1[N:17]=[CH:18][N:19]=[C:20]([O:14][C:10]2[CH:11]=[C:12]([CH3:13])[C:6]3[N:5]=[C:4]([CH2:3][O:2][CH3:1])[NH:8][C:7]=3[CH:9]=2)[CH:21]=1

Komponenten

5

Edukt 3

HCID 11430Potassium CarbonateHCID 709434,6-DichloropyrimidineHCID 669782392-(methoxymethyl)-4-methyl-1H-benzo[d]imidazol-6-ol

Produkt 1

HCID 866639136-(6-chloropyrimidin-4-yloxy)-2-(methoxymethyl)-4-methyl-1H-benzo[d]imidazole

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6228DimethylformamideLösungsmittel

Reaktionsbedingungen

Temperatur
70 °C

Versuchsvorschrift

0.77 g (4.00 mmol) 2-(methoxymethyl)-4-methyl-1H-benzo[d]imidazol-6-ol and 0.68 g (4.40 mmol) 4,6-dichloropyrimidine in 5.0 mL DMF were combined with 1.66 g (12.0 mmol) potassium carbonate and stirred for 8 h at 70° C. Then ice water was added and the substance was extracted with ethyl acetate and concentrated by rotary evaporation i.vac. The residue was purified by preparative HPLC-MS. The fractions containing product were combined and evaporated down i.vac.

Aufarbeitung

  1. extractionthe substance was extracted with ethyl acetate
  2. concentrationconcentrated by rotary evaporation i.vac
  3. customThe residue was purified by preparative HPLC-MS
  4. additionThe fractions containing product
  5. customevaporated down i.vac

Quellen und Nachweise

ORD-Eintrag
ord-55f5ac9dc65742c381a3894364a0fbee
Quelldatensatz
uspto-grants-2015_02
Patentnummer
US08952014B2

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