HRID1944979

反应详情

EQUATION

反应方程式

HRID 1944979 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

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

  1. concentrationthe mixture was concentrated to a residue under reduced pressure
  2. additiontreated successively with TBAF solution (1.0 M in THF, 1 mL) and glacial acetic acid (0.50 mL)
  3. waitThe mixture was left overnight at room temperature
  4. concentrationconcentrated under reduced pressure
  5. customThe residue was purified by reverse-phase high performance liquid chromatography (RP-HPLC, acetonitrile/water/0.1% TFA)
  6. customto provide
  7. concentrationafter concentration