HRID420690

反应详情

EQUATION

反应方程式

HRID 420690 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

A solution of 4-[(1S)-2-{[(1,1-dimethylethyl)(dimethyl)silyl]oxy}-1-(hydroxymethyl)ethyl]-6-(methyloxy)-1,4-dihydropyrido[2,3-b]pyrazin-3(2H)-one (494.1 g, 1.34 mol) and MnO2 (584.4 g, 6.72 mol) in DCM (18 L) was stirred at room temperature for 1 h. The mixture was filtered through celite and the filtrate was evaporated to give a purple/white solid. The crude was purified by column chromatography and mixtures of heptane and EtOAc as eluent to give of 451.6 g (66%) of 4-[(1S)-2-{[(1,1-dimethylethyl)(dimethyl)silyl]oxy}-1-(hydroxymethyl)ethyl]-6-(methyloxy)pyrido[2,3-b]pyrazin-3(4H)-one.

WORKUP

后处理

  1. filtrationThe mixture was filtered through celite
  2. customthe filtrate was evaporated
  3. customto give a purple/white solid
  4. customThe crude was purified by column chromatography and mixtures of heptane and EtOAc as eluent