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
The compound (1.01 g) obtained in Example 29-3, WSCI hydrochloride (973 mg), and HOBt (894 mg) were dissolved in chloroform (30 ml), and the whole was stirred for 2 hours. Then, the compound (445 mg) obtained in Example 29-1 was added thereto and the whole was stirred at room temperature for 3 hours. After completion of the reaction, the solvent was distilled off under reduced pressure. Then, the residue was dissolved in chloroform and washed with a saturated ammonium chloride aqueous solution, a saturated aqueous sodium hydrogen carbonate solution, and a saturated saline solution. After that, the resultant was dried with anhydrous sodium sulfate. After filtration, the solvent was distilled off under reduced pressure. The residue was purified through silica gel column chromatography (chloroform/ethyl acetate), thereby obtaining the subject compound (613 mg) as an orange solid.
WORKUP
后处理
- stirringthe whole was stirred at room temperature for 3 hours
- customAfter completion of the reaction
- distillationthe solvent was distilled off under reduced pressure
- dissolutionThen, the residue was dissolved in chloroform
- washwashed with a saturated ammonium chloride aqueous solution
- dry with materialAfter that, the resultant was dried with anhydrous sodium sulfate
- filtrationAfter filtration
- distillationthe solvent was distilled off under reduced pressure
- customThe residue was purified through silica gel column chromatography (chloroform/ethyl acetate)