HRID1944979
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
Intermediate 158 (90 mg, 0.08 mmol) was taken up in dichloromethane and treated with trifluoroacetic acid (0.50 mL). After 30 minutes of stirring, the mixture was concentrated to a residue under reduced pressure, taken up in tetrahydrofuran (1 mL) and treated successively with TBAF solution (1.0 M in THF, 1 mL) and glacial acetic acid (0.50 mL). The mixture was left overnight at room temperature and then concentrated under reduced pressure. The residue was purified by reverse-phase high performance liquid chromatography (RP-HPLC, acetonitrile/water/0.1% TFA) to provide, after concentration, the trifluoroacetic acid salt of the title compound as a bright yellow foam (22 mg).
WORKUP
后处理
- concentrationthe mixture was concentrated to a residue under reduced pressure
- additiontreated successively with TBAF solution (1.0 M in THF, 1 mL) and glacial acetic acid (0.50 mL)
- waitThe mixture was left overnight at room temperature
- concentrationconcentrated under reduced pressure
- customThe residue was purified by reverse-phase high performance liquid chromatography (RP-HPLC, acetonitrile/water/0.1% TFA)
- customto provide
- concentrationafter concentration