Acetic Acid → 4-Dipropylamino-3-methyl-1,3-dihydroimidazo[4,5-c]pyridin-2-one

Temperatur

45 °C

To a slurry of 750 mg (4.57 mmol) of 4-amino-3-methyl-1,3-dihydroimidazo[4,5-c]pyridin-2-one in 15 mL of dichloroethane was added 3.30 mL (45.7 mmol) of propionaldehyde, 1.0 mL of acetic acid, and 2.90 g (13.7 mmol) of sodium triacetoxyborohydride and the reaction was heated at 45° C. for 7.5 h. The reaction was diluted with 15 mL of dichloromethane and 15 mL of water and the aqueous layer was extracted with 15 mL of dichloromethane. The combined organic layers were dried over sodium sulfate, filtered, and concentrated in vacuo. The residue thus obtained (0.91 g, 80%) was used in the next reaction without further purification.

1. extractionthe aqueous layer was extracted with 15 mL of dichloromethane
2. dry with materialThe combined organic layers were dried over sodium sulfate
3. filtrationfiltered
4. concentrationconcentrated in vacuo
5. customThe residue thus obtained (0.91 g, 80%)
6. customwas used in the next reaction without further purification

ORD-Eintrag

ord-cb882491b8b74f21b97e073eb064ba82

Quelldatensatz

uspto-grants-2010_05

DOI

10.6084/m9.figshare.5104873.v1

Patentnummer

US07714009B2