HRID1895997

反应详情

EQUATION

反应方程式

HRID 1895997 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A well homogenised mixture of the Compound of Example 3 (100 mg, 0.47 mmol), 5-bromo-2-methyl-4-nitro-1H-imidazole (97 mg, 0.47 mmol) and potassium bicarbonate was stirred at 120° C. for 8 h. The reaction mixture was poured into water and extracted with EtOAc The combined organic layers were washed with brine, dried on Na2SO4 and evaporated to dryness in vacuo to afford a residue, which was purified by automated flash liquid chromatography (Horizon™-Biotage), eluting with Petroleum Ether-EtOAc 7:3, affording the title product as a brown solid.

WORKUP

后处理

  1. stirringwas stirred at 120° C. for 8 h
  2. extractionextracted with EtOAc The combined organic layers
  3. washwere washed with brine
  4. customdried on Na2SO4
  5. customevaporated to dryness in vacuo
  6. customto afford a residue, which
  7. customwas purified by automated flash liquid chromatography (Horizon™-Biotage)
  8. washeluting with Petroleum Ether-EtOAc 7:3