反应 #586108

反应方程式

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

收率 84.7%

溶剂

acetic acid

反应条件

后处理

1. 1
   温度the solution was heated
2. 2
   温度under 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
   萃取The aqueous phase was extracted three times with ethyl acetate
6. 6
   干燥the organic phase was dried over sodium sulfate
7. 7
   过滤the drying agent was filtered off
8. 8
   浓缩the filtrate was concentrated to dryness, which

实验过程

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.

来源