Potassium Hydroxide → 2-(3,4-dimethyl-benzyl)-4-oxo-4-[4-(2-oxo-1,4-dihydro-2H-quinazolin-3-yl)-piperidin-1-yl]-butanoic acid

A solution of 15.5 g (28.2 mmol) diethyl 2-(3,4-dimethyl-benzyl)-2-{2-oxo-2-[4-(2-oxo-1,4-dihydro-2H-quinazolin-3-yl)-piperidin-1-yl]-ethyl}-malonate in 100 mL EtOH was combined with 11.2 g (169.7 mmol) KOH dissolved in 150 mL water and the mixture was refluxed for 5 h. After the addition of another 11.2 g (169.7 mmol) KOH dissolved in 150 mL water the mixture was refluxed again for 5 h, then combined with 150 mL water and the precipitate was suction filtered. The filter cake was dissolved in 500 mL water, washed twice with 100 mL EtOAc and adjusted to pH 4 by the addition of conc. HCl. The precipitate formed was suction filtered and dried in the circulating air dryer.

1. temperaturethe mixture was refluxed for 5 h
2. temperaturewas refluxed again for 5 h
3. filtrationfiltered
4. dissolutionThe filter cake was dissolved in 500 mL water
5. washwashed twice with 100 mL EtOAc
6. additionadjusted to pH 4 by the addition of conc. HCl
7. customThe precipitate formed
8. filtrationfiltered
9. customdried in the circulating air dryer

ORD-Eintrag

ord-afcc51205e2942728b9cea1e06f65caa

Quelldatensatz

uspto-grants-2010_04

DOI

10.6084/m9.figshare.5104873.v1

Patentnummer

US07700589B2