HRID35819

反应详情

EQUATION

反应方程式

HRID 35819 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

In 500 ml of chloroform, 50 g of 1-[4-chloro-6-fluoro-3-hydroxy-2-(2 -methyl-2-propenyl)phenyl]-3-methyl-4-trifluoromethyl-1,2,3,6-tetrahydropyrimidine-2,6-dione was dissolved, to which 30.0 g of m-chloroperbenzoic acid was added, and the reaction was effected at 60° C. for 4.5 :hours. After completion of the reaction, the reaction mixture was cooled to room temperature and subjected to fractionation with a separatory funnel using chloroform and an aqueous solution of sodium sulfite. The organic layer was washed with a saturated aqueous solution of sodium hydrogencarbonate and then water, dried and concentrated. The residue was subjected to recrystallization, which afforded 46 g of 1-[4-chloro-6-fluoro-3-hydroxy-2-(2,3-epoxy-2-methylpropyl)phenyl]-3-methyl-4-trifluoromethyl-1,2,3,6-tetrahydropyrimidine-2,6-dione.

WORKUP

后处理

  1. additionwas added
  2. customwas effected at 60° C. for 4.5
  3. customAfter completion of the reaction
  4. customsubjected to fractionation with a separatory funnel
  5. washThe organic layer was washed with a saturated aqueous solution of sodium hydrogencarbonate
  6. dry with materialwater, dried
  7. concentrationconcentrated
  8. customThe residue was subjected to recrystallization, which