Reaktion #325419

Reaktionsgleichung

4-[1-(2-carbamoyl-phenylcarbamoyl)-ethyl]-piperidine-1-carboxylic acid tert-butyl ester

MeONa

→

product

Ausbeute 5.0%

4-[1-(4-oxo-3,4-dihydro-quinazolin-2-yl)-ethyl]-piperidine-1-carboxylic acid tert-butyl ester

Ausbeute 5.0%

Lösungsmittel

MeOH

Reaktionsbedingungen

Aufarbeitung

1. 1
   Temperaturto reflux for 6 hr
2. 2
   Sonstigethe solvent was removed in vacuo
3. 3
   workup.ADDITIONThe residue was diluted with water
4. 4
   Extraktionextracted with EtOAc (300 mL×3)
5. 5
   Trocknenthe organic layer was dried with Na2SO4
6. 6
   Einengenconcentrated
7. 7
   Sonstigepurified by column chromatography

Vorschrift

A solution of 4-[1-(2-carbamoyl-phenylcarbamoyl)-ethyl]-piperidine-1-carboxylic acid tert-butyl ester (20 g, 0.05 mmol, crude from the last step) and MeONa (10 g, 0.19 mol) in MeOH (500 mL) was heated to reflux for 6 hr and the solvent was removed in vacuo. The residue was diluted with water and extracted with EtOAc (300 mL×3), the organic layer was dried with Na2SO4, concentrated and purified by column chromatography to afford the product (2 g, 5%).

Quelle