反応 #2186181

反応方程式

compound ( b44 )

1-chloro-3-ethoxy-2-fluorobenzene

bromine

→

1-bromo-2-chloro-4-ethoxy-3-fluorobenzene

収率 87.9%

反応条件

後処理

1. 1
   workup.ADDITIONwas added dropwise over 1 hour in a temperature range of 20 to 40° C.
2. 2
   その他The resulting reaction mixture
3. 3
   洗浄was washed with a saturated sodium thiosulfate aqueous solution
4. 4
   workup.DISTILLATIONThe residue was subjected to fractional distillation under reduced pressure

実験手順

504 g of the compound (b44) was added to a reactor in a nitrogen atmosphere, to which 434 g of bromine was added dropwise over 1 hour in a temperature range of 20 to 40° C., followed by stirring for 30 minutes. The resulting reaction mixture was washed with a saturated sodium thiosulfate aqueous solution, a 10% sodium hydroxide aqueous solution, and water. The residue was subjected to fractional distillation under reduced pressure to obtain 605 g of 1-bromo-2-chloro-4-ethoxy-3-fluorobenzene (C12). The resulting compound (C12) was white solid and had a melting point of 48.0 to 48.5° C. and a boiling point of 88 to 90° C./1 mmHg.

出典