HRID2424636

反应详情

EQUATION

反应方程式

HRID 2424636 的结构方程式

PROCEDURE

实验过程

The title compound was prepared from D8 and 2-chloropyridine-5-sulfonyl chloride using a method similar to that described for D15 except that the reaction time was overnight. The work-up involved concentration of the reaction mixture and purification by elution through an SCX cartridge (MeOH then 0.2M NH3 in MeOH), followed by column chromatography eluting with 0-20% EtOAc/petroleum ether. δH (CDCl3, 400 MHz) 8.55 (1H, dd), 7.76 (1H, dd), 7.42 (1H, d), 7.21 (1H, d), 6.96 (1H, d), 6.80 (1H, dd), 6.86 (1H, dd), 4.20 (1H, br.s), 3.79 (1H, m), 3.38 (2H, AB), 3.20 (3H, s), 3.05 (1H, m), 2.69 (1H, m), 2.56 (1H, m), 2.32 (3H, s), 2.19 (1H, m), 1.99 (1H, m), 1.46 (9H, s), 1.21 (3H, d). MS (ES+): MH+ 509/511.

WORKUP

后处理

  1. concentrationThe work-up involved concentration of the reaction mixture and purification
  2. washby elution through an SCX cartridge (MeOH
  3. washeluting with 0-20% EtOAc/petroleum ether