反应 #586110

ord-edcec835b10543288395ff8b99605f27

反应方程式

COC(=O)C(C)(C)OC(=O)c1cc(-n2c(=O)cc(C(F)(F)F)n(C)c2=O)c(F)cc1Cl
methyl 2-[2-chloro-5-(3-methyl-2,6-dioxo-4-trifluoromethyl-3,6-dihydro-2H-pyrimidin-1-yl)-4-fluoro-benzoyloxy]-2-methylpropionate
Cl
hydrochloric acid
Cn1c(C(F)(F)F)cc(=O)n(-c2cc(C(=O)OC(C)(C)C(=O)O)c(Cl)cc2F)c1=O
2-[2-chloro-5-(3-methyl-2,6-dioxo-4-trifluoromethyl-3,6-dihydro-2H-pyrimidin-1-yl)-4-fluorobenzoyloxy]-2-methylpropionic acid
收率 68.4%

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 5 hours
  3. 3
    workup.DISTILLATIONMost of the acetic acid was distilled off
  4. 4
    workup.ADDITIONthe solution that remained was poured into ice-water
  5. 5
    过滤The precipitate was filtered off
  6. 6
    其他dried

实验过程

1.0 g (2.1 mmol) of methyl 2-[2-chloro-5-(3-methyl-2,6-dioxo-4-trifluoromethyl-3,6-dihydro-2H-pyrimidin-1-yl)-4-fluoro-benzoyloxy]-2-methylpropionate from example 4.1 was dissolved in 50 ml of acetic acid, 50 ml of conc. hydrochloric acid were added and the reaction mixture was heated under reflux for 5 hours. Most of the acetic acid was distilled off, and the solution that remained was poured into ice-water. The precipitate was filtered off and dried, which gave 0.65 g of 2-[2-chloro-5-(3-methyl-2,6-dioxo-4-trifluoromethyl-3,6-dihydro-2H-pyrimidin-1-yl)-4-fluorobenzoyloxy]-2-methylpropionic acid.

来源

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