反应 #4622

ord-d820998eb2b146de9eeca6c829a21010

反应条件

详细条件
See reaction.notes.procedure_details.

后处理

  1. 1
    温度is refluxed for 4 hours
  2. 2
    其他The semi-liquid reaction mixture
  3. 3
    萃取is extracted 3 to 4 times whilst hot with 1 liter of methanol each time
  4. 4
    浓缩the combined methanol extracts are concentrated by evaporation
  5. 5
    其他the residue is recrystallised from methanol

实验过程

A mixture of 48.2 g of 2,3-dihydro-2,2-dimethyl-6-hydroxy-4H-1,3-benzoxazin-4-one, 70 g of potassium carbonate and 250 ml of 1,2-dibromoethane is refluxed for 4 hours whilst stirring. The semi-liquid reaction mixture is extracted 3 to 4 times whilst hot with 1 liter of methanol each time; the combined methanol extracts are concentrated by evaporation and the residue is recrystallised from methanol. 6-(2-Bromoethoxy)-2,3-dihydro-2,2-dimethyl-4H-1,3-benzoxazin-4-one having a melting point of 190°-195° is obtained.

来源

DOI: 10.6084/m9.figshare.5104873.v1专利: US04727067uspto-grants-1988_02