HRID2366551

反应详情

EQUATION

反应方程式

HRID 2366551 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

Tetrabutylammonium fluoride (0.12 g) was added to a solution of 1-(2-{[tert-butyl(dimethyl)silyl]oxy}ethyl)-3-(1-{(2S)-3-[(6-chloronaphthalen-2-yl)sulfonyl]-2-hydroxypropanoyl}piperidin-4-yl)tetrahydropyrimidin-2(1H)-one (0.25 g) obtained in Example 40c) in THF (10 mL), and the mixture was stirred at room temperature overnight. The solvent was distilled off under reduced pressure, and the residue was diluted with ethyl acetate. The mixture was washed with an aqueous 5% citric acid solution and saturated saline solution, dried over anhydrous magnesium sulfate and then concentrated under reduced pressure. The residue was purified by basic silica gel column chromatography (ethyl acetate/methanol=95/5 to ethyl acetate/methanol=90/10) to obtain the title compound (0.11 g, 54%) as a white powder.

WORKUP

后处理

  1. distillationThe solvent was distilled off under reduced pressure
  2. additionthe residue was diluted with ethyl acetate
  3. washThe mixture was washed with an aqueous 5% citric acid solution and saturated saline solution
  4. dry with materialdried over anhydrous magnesium sulfate
  5. concentrationconcentrated under reduced pressure
  6. customThe residue was purified by basic silica gel column chromatography (ethyl acetate/methanol=95/5 to ethyl acetate/methanol=90/10)