HRID1840620
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
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
- customThe methanol was then removed in vacuo
- concentrationthe mixture was concentrated in vacuo
- customThe residue was chromatographed over silica gel
- concentrationAfter concentrating the product fractions
- customdried