HRID2237464

反应详情

EQUATION

反应方程式

HRID 2237464 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

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

  1. additioncontaining
  2. temperatureat reflux for 1 hour
  3. customevaporated to a brown oil
  4. customThe crude reaction product
  5. customwas purified by flash chromatography (SiO2, 3-30% ethyl acetate/hexanes)