HRID1963068
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 the compound of step 1 (2.52 g, 6.66 mmol) in 45 ml of acetone were added potassium carbonate (5.522 g, 39.96 mmol) and iodomethane (1.24 ml, 19.98 mmol) and the solution was stirred at room temperature overnight. The mixture was filtered and the filtrate was concentrated to dryness. The residue was dissolved in EA, washed twice with brine, dried over sodium sulfate, filtered and evaporated under reduced pressure. The residue was purified by chromatography on silica gel (cyclohexane/EA, 100:0, then 85:15) to give 2.334 g of the title compound as a colorless oil.
WORKUP
后处理
- filtrationThe mixture was filtered
- concentrationthe filtrate was concentrated to dryness
- dissolutionThe residue was dissolved in EA
- washwashed twice with brine
- dry with materialdried over sodium sulfate
- filtrationfiltered
- customevaporated under reduced pressure
- customThe residue was purified by chromatography on silica gel (cyclohexane/EA, 100:0