反応 #64097

反応方程式

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

m-chloroperbenzoic acid

sodium sulfite

→

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

収率 88.4%

溶媒

chloroform

chloroform

反応条件

後処理

1. 1
   workup.ADDITIONwas added
2. 2
   その他was effected at 60° C. for 4.5
3. 3
   その他After completion of the reaction
4. 4
   その他subjected to fractionation with a separatory funnel
5. 5
   洗浄The organic layer was washed with a saturated aqueous solution of sodium hydrogencarbonate
6. 6
   乾燥water, dried
7. 7
   濃縮concentrated
8. 8
   その他The residue was subjected to recrystallization, which

実験手順

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.

出典