HRID1840620

反应详情

EQUATION

反应方程式

HRID 1840620 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

0.82 mL (0.82 mmol) of a 1 M aqueous lithium hydroxide solution was added to a solution of 141 mg (0.206 mmol) of the compound of Example 9 in 7.25 mL of methanol and the reaction mixture was allowed to stand overnight at room temperature. The methanol was then removed in vacuo, the residue was adjusted to pH 2 using 1N hydrochloric acid and the mixture was concentrated in vacuo. The residue was chromatographed over silica gel using dichloromethane/methanol/glacial acetic acid/water (95/5/0.5/0.5). After concentrating the product fractions, the residue was treated with 1.11 equivalents of 1N hydrochloric acid and freeze dried. Yield: 120 mg (89%).

WORKUP

后处理

  1. customThe methanol was then removed in vacuo
  2. concentrationthe mixture was concentrated in vacuo
  3. customThe residue was chromatographed over silica gel
  4. concentrationAfter concentrating the product fractions
  5. customdried