HRID1480777

反应详情

EQUATION

反应方程式

HRID 1480777 反应方程式

PROCEDURE

实验过程

The title compound was prepared according to Example 40 using N-(4-(1,2-dimethyl-1H-imidazol-5-yl)-2-methoxyphenyl)formamide (Preparation 55) and 2-(methylsulfonyl)-N-neopentylpyrido[3,4-d]pyrimidin-8-amine (Preparation 47). The residue was purified by silica gel column chromatography eluting with 0-10% MeOH in EtOAc. The residue was purified by passage through a SCX-2 cartridge eluting with 100% MeOH-1M NH3 in MeOH. The residue was diluted with DCM (30 mL) and washed with 0.1M HCl (30 mL), dried (MgSO4) and concentrated in vacuo. The residue was further purified by SCX-2 cartridge eluting with 100% MeOH-1M NH3 in MeOH followed by silica gel column chromatography eluting with 0-7% MeOH in EtOAc to give the title compound (5.5 mg, 21%).

WORKUP

后处理

  1. customThe title compound was prepared
  2. customThe residue was purified by silica gel column chromatography
  3. washeluting with 0-10% MeOH in EtOAc
  4. customThe residue was purified by passage through a SCX-2 cartridge
  5. washeluting with 100% MeOH-1M NH3 in MeOH
  6. additionThe residue was diluted with DCM (30 mL)
  7. washwashed with 0.1M HCl (30 mL)
  8. dry with materialdried (MgSO4)
  9. concentrationconcentrated in vacuo
  10. customThe residue was further purified by SCX-2 cartridge
  11. washeluting with 100% MeOH-1M NH3 in MeOH
  12. washeluting with 0-7% MeOH in EtOAc