反应 #586109

ord-48355419a8f7424db5fb3502e70167b0

反应方程式

C[C@H](OC(=O)c1cc(-n2c(=O)cc(C(F)(F)F)n(C)c2=O)ccc1Cl)C(=O)O
(S)-2-[2-chloro-5-(3-methyl-2,6-dioxo-4-trifluoromethyl-3,6-dihydro-2H-pyrimidin-1-yl)benzoyloxy]-propionic acid
O=S(Cl)Cl
thionyl chloride
C[C@H](OC(=O)c1cc(-n2c(=O)cc(C(F)(F)F)n(C)c2=O)ccc1Cl)C(=O)Cl
(S)-2-[2-chloro-5-(3-methyl-2,6-dioxo-4-trifluoromethyl-3,6-dihydro-2H-pyrimidin-1-yl)-benzoyloxy]propionyl chloride

反应条件

详细条件
See reaction.notes.procedure_details.

后处理

  1. 1
    温度the reaction mixture was heated
  2. 2
    温度under reflux for 3.5 hours
  3. 3
    温度to cool
  4. 4
    浓缩concentrated

实验过程

5.7 g (14 mmol) of (S)-2-[2-chloro-5-(3-methyl-2,6-dioxo-4-trifluoromethyl-3,6-dihydro-2H-pyrimidin-1-yl)benzoyloxy]-propionic acid from example 3.2 were dissolved in 50 ml of thionyl chloride, and the reaction mixture was heated under reflux for 3.5 hours. The solution was allowed to cool and concentrated, which gave 5.9 g of (S)-2-[2-chloro-5-(3-methyl-2,6-dioxo-4-trifluoromethyl-3,6-dihydro-2H-pyrimidin-1-yl)-benzoyloxy]propionyl chloride.

来源

DOI: 10.6084/m9.figshare.5104873.v1专利: US07767624B2uspto-grants-2010_08