HRID2203103
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
To a solution of (4-(trifluoromethyl)thiophen-2-yl)methanol (50 mg) in THF (3 ml) were added 1-(2-ethyl-1-methyl-1H-benzo[d]imidazol-6-yl)-4-hydroxypyridin-2(1H)-one (73.9 mg), bis(2-methoxyethyl) azodicarboxylate (129 mg) and PPh3 (144 mg) at room temperature, and the mixture was stirred for 3 h. The mixture was poured into water and extracted with EtOAc. The organic layer was separated, washed with saturated NaHCO3 solution and brine successively, dried over MgSO4 and concentrated in vacuo. The residue was purified by column chromatography (EtOAc/MeOH) to give the title compound (10.2 mg) as white crystals.
WORKUP
后处理
- extractionextracted with EtOAc
- customThe organic layer was separated
- washwashed with saturated NaHCO3 solution and brine successively
- dry with materialdried over MgSO4
- concentrationconcentrated in vacuo
- customThe residue was purified by column chromatography (EtOAc/MeOH)