تفاعل #586108

معادلة التفاعل

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

المردود 84.7%

المذيبات

acetic acid

ظروف التفاعل

المعالجة

1. 1
   درجة الحرارةthe solution was heated
2. 2
   درجة الحرارةunder 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
   استخلاصThe aqueous phase was extracted three times with ethyl acetate
6. 6
   تجفيفthe organic phase was dried over sodium sulfate
7. 7
   ترشيحthe drying agent was filtered off
8. 8
   تركيزthe filtrate was concentrated to dryness, which

الإجراء التجريبي

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.

المصدر