反応 #1455201

反応方程式

3-(2-amino-4-chloro-6-fluoro-3-hydroxyphenyl)-1-methyl-6-trifluoromethyl-2,4(1H,3H)-pyrimidinedione

phenacyl bromide

potassium carbonate

→

title compound

収率 18.7%

3-(8-Chloro-6-fluoro-3-phenyl-2H-1,4-benzoxazin-5-yl)-1-methyl-6-trifluoromethyl-2,4(1H,3H)-pyrimidindione

収率 18.7%

溶媒

acetone

反応条件

後処理

1. 1
   その他Then insoluble salt was removed through Celite
2. 2
   濃縮the filtrate concentrated under reduced pressure
3. 3
   その他The oily substance was purified by column chromatography on silica gel

実験手順

A mixture of 3-(2-amino-4-chloro-6-fluoro-3-hydroxyphenyl)-1-methyl-6-trifluoromethyl-2,4(1H,3H)-pyrimidinedione (0.5 g), phenacyl bromide (0.29 g) and potassium carbonate (0.2 g) in acetone (30 ml) was stirred under reflux conditions for 1 hour. Then insoluble salt was removed through Celite and the filtrate concentrated under reduced pressure. The oily substance was purified by column chromatography on silica gel using ethyl acetate-hexane(1:4) as eluent to give the title compound (0.12 g).

出典