反応 #78995

反応方程式

8-fluoro-4,4-dimethyl-dihydro-benzo[d][1,3]oxazin-2-one

bromine

→

6-bromo-8-fluoro-4,4-dimethyl-dihydro-benzo[d][1,3]oxazin-2-one

収率 84.0%

溶媒

acetic acid

acetic acid

反応条件

後処理

1. 1
   濃縮the mixture was concentrated
2. 2
   その他the residue obtained
3. 3
   その他was purified by a silica gel column (hexane:ethyl acetate/4:1)

実験手順

To a solution of 8-fluoro-4,4-dimethyl-dihydro-benzo[d][1,3]oxazin-2-one (0.15 g, 0.77 mmol) in acetic acid (5 mL) was added dropwise a solution of bromine (0.37 g, 2.31 mmol) in acetic acid (5 mL) under nitrogen at rt. After stirring for 10 minutes, the mixture was concentrated and the residue obtained was purified by a silica gel column (hexane:ethyl acetate/4:1) to afford 6-bromo-8-fluoro-4,4-dimethyl-dihydro-benzo[d][1,3]oxazin-2-one as an off-white solid (0.176 g, 84%) which was used in next step without further purification.

出典