反应 #1949412

ord-c1a1f95af5e040f88a159a5c5575daf5

反应条件

详细条件
See reaction.notes.procedure_details.

后处理

  1. 1
    workup.ADDITIONwas added to the mixture
  2. 2
    workup.STIRRINGthe mixture was stirred at 50° C. for 1 hour
  3. 3
    浓缩the filterate was concentrated under reduced pressure

实验过程

To a mixture of 0.10 g of 3-{2-chloro-4-fluoro-5-[2,6-dioxo-4-(trifluoromethyl)-1,2,3,6-tetrahydropyrimidin-1-yl]phenoxy}-2-(methoxycarbonyl)methoxypyridine, 1 ml of acetonitrile and 31 mg of potassium carbonate, 32 mg of methyl iodide was added to the mixture, and the mixture was stirred at room temperature for 1.5 hours. 64 mg of methyl iodide was added to the mixture, and the mixture was stirred at 50° C. for 1 hour. The mixture was filterated, and the filterate was concentrated under reduced pressure. The residue was subjected to silica gel column chromatography to obtain 97 mg of 3-{2-chloro-4-fluoro-5-[3-methyl-2,6-dioxo-4-(trifluoromethyl)-1,2,3,6-tetrahydropyrimidin-1-yl]phenoxy}-2-(methoxycarbonyl)methoxypyridine [present compound 7-7].

来源

DOI: 10.6084/m9.figshare.5104873.v1专利: US06537948B1uspto-grants-2003_03