HRID1862237

反应详情

EQUATION

反应方程式

HRID 1862237 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

0.40 g of 2-chloro-4-fluoro-5-[3-methyl-2,6-dioxo-4-(trifluoromethyl)-1,2,3,6-tetrahydropyrimidin-1-yl]phenyl mercaptan was dissolved in 6 ml of acetonitrile, to this solution was added 0.31 g of potassium carbonate, and the mixture was stirred for 30 minutes, then, 0.29 g of 2-chloro-4-[1-(methoxycarbonyl)ethoxy]pyrimidine was added and the mixture was stirred for 3 hours. This reaction solution was poured into ice water, and extracted with ethyl acetate. The organic layer was washed with saturated saline, dried over anhydrous magnesium sulfate, and concentrated. The residue was subjected to silica gel column chromatography to obtain 0.46 g of methyl 2-([2-{2-chloro-4-fluoro-5-[3-methyl-2,6-dioxo-4-(trifluoromethyl)-1,2,3,6-tetrahydropyrimidin-1-yl]phenylthio}pyrimidin-4-yl]oxy}propionate [present compound 6-2].

WORKUP

后处理

  1. stirringthe mixture was stirred for 3 hours
  2. extractionextracted with ethyl acetate
  3. washThe organic layer was washed with saturated saline
  4. dry with materialdried over anhydrous magnesium sulfate
  5. concentrationconcentrated