HRID545376
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 0.52 g (1.00 mmol) of [2-(3-hexyl-phenyl)-3-methyl-5-trimethylsilanylethynyl-3H-imidazol-4-yl]-(4-pyrrolidin-1-yl-piperidin-1-yl)-methanone (example 12) in 10 ml EtOH:THF 5:1 was added 0.277 g (2.0 mmol) of solid potassium carbonate and the reaction mixture was stirred at RT for 18 hours. It was then poured into crashed ice, acidified with HCl (25% in water) and extracted twice with CH2Cl2; the organic phases were washed with water, dried over magnesium sulfate, filtered and evaporated. The residue was purified by flash column chromatography (CH2Cl2/MeOH 1:0 to 9:1) to give 0.27 g (60%) of the title compound as light brown solid. MS: 447.4 (MH+).
WORKUP
后处理
- additionIt was then poured
- extractionextracted twice with CH2Cl2
- washthe organic phases were washed with water
- dry with materialdried over magnesium sulfate
- filtrationfiltered
- customevaporated
- customThe residue was purified by flash column chromatography (CH2Cl2/MeOH 1:0 to 9:1)