HRID567676

反应详情

EQUATION

反应方程式

HRID 567676 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

5-Acetamidoanthranilic acid (0.64g) and 2,6-difluorobenzoyl chloride (1.3 g) were reacted in triethyl amine/toluene (1/1) (20 mL) like described for compound (9), reaction time 1 h. Ethyl acetate (50 mL) and HCl-solution (1 mL 4N in 50 mL water) were added resulting in the formation of a precipitate.The mixture was filtered and the residue dissolved in THF followed by evaporation to dryness, subsequent dissolution in hot dioxane followed by precipitation with hexane resulted in colourless crystals of 6-acetamido-(2,6-difluoro-phenyl)-benzo[d][1,3]oxazin-4-one (0.98 g), mp.246 C, MS m/e.: 316 M+.

WORKUP

后处理

  1. customresulting in the formation of a precipitate.The mixture
  2. filtrationwas filtered
  3. dissolutionthe residue dissolved in THF
  4. customfollowed by evaporation to dryness, subsequent dissolution in hot dioxane
  5. customfollowed by precipitation with hexane