HRID1895997
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
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
- stirringwas stirred at 120° C. for 8 h
- extractionextracted with EtOAc The combined organic layers
- washwere washed with brine
- customdried on Na2SO4
- customevaporated to dryness in vacuo
- customto afford a residue, which
- customwas purified by automated flash liquid chromatography (Horizon™-Biotage)
- washeluting with Petroleum Ether-EtOAc 7:3