HRID648752

反应详情

EQUATION

反应方程式

HRID 648752 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A suspension of 20.3 g of 2-chloro-butyryl chloride and 12.3 g of 2-amino-3-trifluoromethyl-benzoic acid in toluene was refluxed under reduced pressure for one hour and was then evaporated to dryness under reduced pressure. The oil residue was added to 100 ml of iced water and the mixture was stirred for one hour and was vacuum filtered. The product was washed with water and dried under reduced pressure at 50° C. to obtain 17 g of 2-(1-chloropropyl)-8-trifluoromethyl-4H-3,1-benzoxazine-4-one melting at 65°-70° C.

WORKUP

后处理

  1. temperaturewas refluxed under reduced pressure for one hour
  2. customwas then evaporated to dryness under reduced pressure
  3. additionThe oil residue was added to 100 ml of iced water
  4. filtrationfiltered
  5. washThe product was washed with water
  6. customdried under reduced pressure at 50° C.