HRID1662481
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 66.63A (0.322 mmol) in DMF (4 mL), was added NaH (0.0100 g, 0.419 mmol). The resulting mixture was stirred at room temperature for 10 minutes. 1-Bromo-3-methylbut-2-ene (0.240 g, 1.61 mmol) (commercially available from Aldrich) was added and the mixture was stirred at room temperature for 2 hours. After removing solvent, the residue was purified by flash chromatography (silica gel, 1:6 EtOAc/hexane) and gave 67.27A as a colorless oil, in 77% yield. MS ESI (pos.) m/e: 430 (M+18)+.
WORKUP
后处理
- stirringthe mixture was stirred at room temperature for 2 hours
- customAfter removing solvent
- customthe residue was purified by flash chromatography (silica gel, 1:6 EtOAc/hexane)