Reaktion #2288377

Reaktionsgleichung

methyl 3-(1,3-dimethyl-2,4-dioxo-5-phenyl-3,4-dihydro-1H-pyrrolo[3,4-d]pyrimidin-6(2H)-yl)propanoate

water

LiOH

→

3-(1,3-Dimethyl-2,4-dioxo-5-phenyl-3,4-dihydro-1H-pyrrolo[3,4-d]pyrimidin-6(2H)-yl)propanoic acid

Lösungsmittel

THF

EtOAc

Reaktionsbedingungen

Aufarbeitung

1. 1
   Sonstigethe layers separated
2. 2
   WaschenThe organics were then washed with water (3×50 ml)
3. 3
   SonstigeThe resulting precipitate was isolated
4. 4
   Filtrationsuction filtration

Vorschrift

A mixture of methyl 3-(1,3-dimethyl-2,4-dioxo-5-phenyl-3,4-dihydro-1H-pyrrolo[3,4-d]pyrimidin-6(2H)-yl)propanoate (step 2) (3.24 g, 9.49 mmol) in THF (33.9 mL)/water (33.9 mL) and LiOH (2.273 g, 95 mmol) was heated to 50° C. for 1 hr. The reaction mixture was diluted with EtOAc (50 ml) and the layers separated. The organics were then washed with water (3×50 ml). The aqueous extracts were combined and the pH adjusted to approx. pH3 with 5M HCl. The resulting precipitate was isolated using suction filtration.

Quelle