HRID2259996
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
Ethyl (E)-4-[2-(5,6,7,8 -tetrahydro-3,5,5,8,8-pentamethylnaphthalen-2-yl)propen-1-yl]-1-N,N-dimethylsulfamoyl-2-imidazolecarboxylate (Compound 4, 70 mg, 0.18 mmol) was dissolved in acetone (10 mL) at room temperature and treated with methyl iodide (0.5 mL) and K2CO3 (350 mg). The suspension was stirred for 30 min, filtered through Celite and concentrated under reduced pressure. The residue was treated with water (5 mL) and the organic material was extracted with ethyl acetate, washed with brine, dried (MgSO4) and concentrated in vacuo. The residue was purified by flash chromatography on silica gel (hexanes/ethyl acetate=5:1) to give the title compound as a light yellow solid (35 mg, 50%).
WORKUP
后处理
- filtrationfiltered through Celite
- concentrationconcentrated under reduced pressure
- additionThe residue was treated with water (5 mL)
- extractionthe organic material was extracted with ethyl acetate
- washwashed with brine
- dry with materialdried (MgSO4)
- concentrationconcentrated in vacuo
- customThe residue was purified by flash chromatography on silica gel (hexanes/ethyl acetate=5:1)