HRID60686

反应详情

EQUATION

反应方程式

HRID 60686 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

A solution of Intermediate 78c (60.0 mg, 0.08 mmol) and pyridinium p-toluene sulphonate (58.0 mg, 0.23 mmol) in MeOH (1 mL) was heated at 45° C. for 18 h. The reaction mixture was cooled and diluted with DCM (5 mL). This was washed with sat. aq. NaHCO3 (2×5 mL). The organic layer was passed through a phase separator and concentrated in vacuo. The residue was purified by FCC, using 0-10% MeOH in DCM, to afford the title compound (42 mg, 78%). LCMS (Method 3): Rt: 3.47 min, m/z 699/701 [MH+].

WORKUP

后处理

  1. temperatureThe reaction mixture was cooled
  2. washThis was washed with sat. aq. NaHCO3 (2×5 mL)
  3. concentrationconcentrated in vacuo
  4. customThe residue was purified by FCC