Реакция #586108

Уравнение реакции

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

Выход 84.7%

Растворители

acetic acid

Условия реакции

Обработка

1. 1
   Температураthe solution was heated
2. 2
   Температураunder 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
   ЭкстракцияThe aqueous phase was extracted three times with ethyl acetate
6. 6
   Сушкаthe organic phase was dried over sodium sulfate
7. 7
   Фильтрацияthe drying agent was filtered off
8. 8
   Концентрированиеthe filtrate was concentrated to dryness, which

Методика

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.

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