HRID1822465

反应详情

EQUATION

反应方程式

HRID 1822465 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

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

  1. customwas taken up to ambient temperature
  2. concentrationAfter 10 min the resulting mixture was concentrated
  3. dissolutionre-dissolved in ethyl acetate
  4. washwashed with K2CO3 (aq)
  5. customDried
  6. concentrationconcentrated which