Reaktion #586108

Reaktionsgleichung

methyl (S)-2-[2-chloro-5-(3-methyl-2,6-di-oxo-4-trifluoromethyl-3,6-dihydro-2H-pyrimidin-1-yl)benzoyl-oxy]propionate

hydrochloric acid

→

(S)-2-[2-chloro-5-(3-methyl-2,6-dioxo-4-trifluoromethyl-3,6-dihydro-2H-pyrimidin-1-yl)benzoyloxy]propionic acid

Ausbeute 84.7%

Lösungsmittel

acetic acid

Reaktionsbedingungen

Aufarbeitung

1. 1
   Temperaturthe solution was heated
2. 2
   Temperaturunder reflux for 4 hours
3. 3
   workup.DISTILLATIONMost of the acetic acid was distilled off
4. 4
   workup.ADDITIONthe solution that remained was poured onto ice-water
5. 5
   ExtraktionThe aqueous phase was extracted three times with ethyl acetate
6. 6
   Trocknenthe organic phase was dried over sodium sulfate
7. 7
   Filtrationthe drying agent was filtered off
8. 8
   Einengenthe filtrate was concentrated to dryness, which

Vorschrift

7.0 g (16 mmol) of methyl (S)-2-[2-chloro-5-(3-methyl-2,6-di-oxo-4-trifluoromethyl-3,6-dihydro-2H-pyrimidin-1-yl)benzoyl-oxy]propionate from example 3.1 were dissolved in 50 ml of acetic acid, 50 ml of conc. hydrochloric acid were added and the solution was heated under reflux for 4 hours. Most of the acetic acid was distilled off, and the solution that remained was poured onto ice-water. The aqueous phase was extracted three times with ethyl acetate, the organic phase was dried over sodium sulfate, the drying agent was filtered off and the filtrate was concentrated to dryness, which gave 5.7 g of (S)-2-[2-chloro-5-(3-methyl-2,6-dioxo-4-trifluoromethyl-3,6-dihydro-2H-pyrimidin-1-yl)benzoyloxy]propionic acid.

Quelle