HRID2237464
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 solution of 2-{[(3-{[tert-butyl(diphenyl)silyl]oxy}propyl)amino]methyl}aniline (0.45 g, 1.1 mmol) and sulfamide (0.12 g, 1.3 mmol) in diglyme (5 mL) was added dropwise to a flask containing refluxing diglyme (3 mL) over 10 minutes. The reaction mixture was stirred at reflux for 1 hour, then cooled to room temperature and evaporated to a brown oil. The crude reaction product was purified by flash chromatography (SiO2, 3-30% ethyl acetate/hexanes) to afford 3-(3-{[tert-butyl(diphenyl)silyl]oxy}propyl)-3,4-dihydro-1H-2,1,3-benzothiadiazine 2,2-dioxide (0.50 g, 95%) as a colorless oil:
WORKUP
后处理
- additioncontaining
- temperatureat reflux for 1 hour
- customevaporated to a brown oil
- customThe crude reaction product
- customwas purified by flash chromatography (SiO2, 3-30% ethyl acetate/hexanes)