HRID964949

反应详情

EQUATION

反应方程式

HRID 964949 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture of 2-(3-chloropropyl)-2H-1,2-benzothiazin-4(3H)-one 1,1-dioxide ethylene ketal (5.0 g, 15.7 mmol.), 3N aqueous hydrochloric acid (30 mL) and methanol (30 mL) was heated under refluxing for 20 min. Methanol was distilled off under reduced pressure. To the residue was added water (30 mL), and the mixture was extracted with ethyl ether. The ethyl ether portion was washed with an aqueous saturated sodium chloride solution, dried over anhydrous sodium sulfate, and placed under reduced pressure to distill the solvent off, to give the desired compound (4.19 g, 100%) as a yellow oil.

WORKUP

后处理

  1. temperaturewas heated
  2. temperatureunder refluxing for 20 min
  3. distillationMethanol was distilled off under reduced pressure
  4. additionTo the residue was added water (30 mL)
  5. extractionthe mixture was extracted with ethyl ether
  6. washThe ethyl ether portion was washed with an aqueous saturated sodium chloride solution
  7. dry with materialdried over anhydrous sodium sulfate
  8. distillationto distill the solvent off,