HRID1257096

反应详情

EQUATION

反应方程式

HRID 1257096 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
25 °C

PROCEDURE

实验过程

0.085 mL of sulfuric acid (concentrate, 1.1 equiv) was added into the mixture of 1 g of atazanavir base, 7.5 mL of EtOH (7.5 vol) and 7.5 mL of MTBE (7.5 vol) at 20-30° C. The resulting clear amber solution was stirred at 20-30° C. for 4 hr. The product was filtered, washed with a mixture of EtOH/MTBE (1:2, 3 mL, 3 vol), and dried under vacuum at 40-50° C. for 16 hr to afford atazanavir sulfate in Form A (1.04 g, 91% yield, 99.9% HPLC purity).

WORKUP

后处理

  1. filtrationThe product was filtered
  2. washwashed with a mixture of EtOH/MTBE (1:2, 3 mL, 3 vol)
  3. customdried under vacuum at 40-50° C. for 16 hr