HRID1822465
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
To a stirred solution of compound 89 (1.81 g) in acetonitrile at 0° C. solid NaHCO3 (800 mg) and p-nitrophenychlorocarbonate (1.2 g) was added. The slurry was taken up to ambient temperature and stirred for another 30 min. To this slurry a solution of compound 91 (1.6 g) in acetonitrile (5 mL) diisopropylethylamine (1 mL) was added. After 10 min the resulting mixture was concentrated, re-dissolved in ethyl acetate and washed with K2CO3 (aq) and then with 0.5 N HCl. Dried and concentrated which gave a >80% pure product by HPLC M+H+599.6
WORKUP
后处理
- customwas taken up to ambient temperature
- concentrationAfter 10 min the resulting mixture was concentrated
- dissolutionre-dissolved in ethyl acetate
- washwashed with K2CO3 (aq)
- customDried
- concentrationconcentrated which