HRID964949
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
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
- temperaturewas heated
- temperatureunder refluxing for 20 min
- distillationMethanol was distilled off under reduced pressure
- additionTo the residue was added water (30 mL)
- extractionthe mixture was extracted with ethyl ether
- washThe ethyl ether portion was washed with an aqueous saturated sodium chloride solution
- dry with materialdried over anhydrous sodium sulfate
- distillationto distill the solvent off,