HRID876589

反应详情

EQUATION

反应方程式

HRID 876589 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

CONDITIONS

反应条件

温度
0 °C

PROCEDURE

实验过程

To a solution of compound 70-2 (80 mg) in CH2Cl2 (2 ml) at 0° C. was added pyridine (26 μL), Ac2O (30 μl), and DMAP (4 mg). The mixture was stirred for 1 hour at 0° C., warmed to rt, and stirred for an additional 12 h. The mixture was diluted with EtOAc and the organic layer was washed sequentially with sat. aq. CuSO4 solution, water, and brine. The organic layer was dried (Na2SO4), filtered, and concentrated under reduced pressure to afford compound 70-3 (85 mg) as a light yellow semisolid. LC-MS: M+H=419. This material was used without further purification.

WORKUP

后处理

  1. temperaturewarmed to rt
  2. stirringstirred for an additional 12 h
  3. washthe organic layer was washed sequentially with sat. aq. CuSO4 solution, water, and brine
  4. dry with materialThe organic layer was dried (Na2SO4)
  5. filtrationfiltered
  6. concentrationconcentrated under reduced pressure