HRID1036994

反应详情

EQUATION

反应方程式

HRID 1036994 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
50 °C

PROCEDURE

实验过程

182 mg (0.50 mmol) of the compound from Example 17A are provided in 2 ml of dioxane, and 4.4 ml (8.80 mmol) of a 2N aqueous lithium hydroxide solution are added. The mixture is stirred at 50° C. for 2 hours and subsequently concentrated. The residue is diluted with water, a concentrated aqueous HCl solution is added until an acidic pH is obtained and the mixture is extracted with dichloromethane. The organic phase is dried over magnesium sulfate, filtered and concentrated. The crude product is purified by preparative HPLC (RP18 column; eluent: acetonitrile/water gradient). 159 mg (95% of theory) of the title compound are obtained.

WORKUP

后处理

  1. concentrationsubsequently concentrated
  2. additionThe residue is diluted with water
  3. additiona concentrated aqueous HCl solution is added until an acidic pH
  4. customis obtained
  5. extractionthe mixture is extracted with dichloromethane
  6. dry with materialThe organic phase is dried over magnesium sulfate
  7. filtrationfiltered
  8. concentrationconcentrated
  9. customThe crude product is purified by preparative HPLC (RP18 column; eluent: acetonitrile/water gradient)