摘要
将2.0 mmoL炔基溴化镁在5.0 mL THF的溶液冷却到0℃,加入无水ZnCl2（2.0 mmoL）及无水THF 10 mL,加热升温到室温搅拌30 min,然后加入干燥研细的硒粉（2.0 mmoL）,加热回流直到硒粉完全消失,加入二芳基碘盐（2.0 mmoL）及无水HMPA 5.0mL,在60℃搅拌5 h,用稀盐酸稀释,乙醚（3×50 mL）萃取,将有机相旋转去掉溶剂后的剩余物通过柱层析纯化,用石油醚/乙醚（30/1）作洗脱剂.收率为72%-83%.
To the solution of alkynyl magnesium bromide （2.0 mmoL） in 5.0 mL was added anhydrous zinc chloride （2.0 mmoL） and 10.0 mL THF at 0 ℃. The mixture was stirred at room temperature for 30 minutes, and then dry power selenium （2.0 mmoL） was added to the solution, which was stirred in boiling THF till the selenium disappeared. To the solution was added the diaryliodonium salt （2.0 mmoL） and dry HMPA （5.0 mL）, and the mixture was stirred for 5 h at 60 ℃. It was diluted with dilute aqueous HCl （20 mL）, and the aqueous layer was extracted with ether （3 × 20 mL）. The combined organic phase was washed with a saturated aqueous Na2CO3 solution solution and brine respectively, and dried （MgSO4）, and then the solvent was evaporated. The reside was subjected to column chromatography using light petroleum-ether as eluent （30：1） to afford the aryl alkynyl selenides in yields 72 % - 83 %.
出处
《湖南大学学报（自然科学版）》
EI
CAS
CSCD
北大核心
2008年第2期70-72,共3页
Journal of Hunan University:Natural Sciences
基金
国家自然科学基金资助项目(20372020)
关键词
硒粉
芳基炔硒醚
插入反应
selenium
aryl alkynyl selenides
insertion reaction
作者简介
许新华（1964-），男，湖南武冈人，教授，从事有机合成研究 通讯联系人，E．mail：xhx1581@yahoo．com.cn
