HRID463061

反应详情

EQUATION

反应方程式

HRID 463061 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A solution of 19.3 gm (0.1 mol) of 6-hydroxy-4,4-dimethyl-4H-3,1-benzoxazin-2-one in 200 ml of dimethyl sulfoxide is mixed at ambient temperature with 41.5 gm (0.3 mol) of potassium carbonate and 92 gm (0.4 mol) of 1,5-dibromopentane, whereupon the temperature rises to 45° C. After stirring a further two hours, ice water is added, and the resulting mixture is extracted with chloroform. The chloroform phase is washed with water and dried with sodium sulfate, and the chloroform is distilled off. The residue is recrystallized from ethyl acetate/petroleum ether.

WORKUP

后处理

  1. customrises to 45° C
  2. extractionthe resulting mixture is extracted with chloroform
  3. washThe chloroform phase is washed with water
  4. dry with materialdried with sodium sulfate
  5. distillationthe chloroform is distilled off
  6. customThe residue is recrystallized from ethyl acetate/petroleum ether