反応 #4644

ord-152204720d674800a0350d569265abe5

反応条件

詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    ろ過The reaction mixture is filtered
  2. 2
    温度whilst warm
  3. 3
    濃縮the filtrate is concentrated by evaporation
  4. 4
    ろ過the remaining crystals are suction-filtered after trituration with ether

実験手順

A solution of 9.65 g of 2,3-dihydro-2,2-dimethyl-6-hydroxy-4H-1,3-benzoxazin-4-one and 9.1 g of allyl bromide in 150 ml of acetonitrile is refluxed for 5 hours, whilst stirring, with the addition of 10.3 g of dry potassium carbonate. The reaction mixture is filtered whilst warm, the filtrate is concentrated by evaporation and the remaining crystals are suction-filtered after trituration with ether. The crude 2,3-dihydro-2,2-dimethyl-6-(1-propen-3-yloxy)-4H-1,3-benzoxazin-4-one obtained in this manner melts at 137°-138°.

出典

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