HRID903131

反应详情

EQUATION

反应方程式

HRID 903131 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

The oxalic acid salt of 3-(4-trifluoromethylphenoxy) azetidine (13.0 g., 0.042 mole) was partitioned between 50 ml. of benzene and 50 ml. of potassium hydroxide solution. The benzene layer was dried over calcium sulfate and filtered, and to the stirring dried benzene solution was added 2.6 g. (0.046 mole) of methyl-isocyanate. Stirring was continued overnight. The mixture was concentrated at reduced pressure and the solid residue was recrystallized from a mixture of isopropyl ether-ethyl acetate. The product weighed 7.5 g. (65%) and melted at 154°-157° C.

WORKUP

后处理

  1. dry with materialThe benzene layer was dried over calcium sulfate
  2. filtrationfiltered
  3. additionto the stirring dried benzene solution was added 2.6 g
  4. concentrationThe mixture was concentrated at reduced pressure
  5. customthe solid residue was recrystallized from a mixture of isopropyl ether-ethyl acetate