以可回收的I2/PEG400型离子液体(I2/IL400)为催化体系,发展了一种高效、实用的合成全乙酰糖衍生物的方法.结果表明,以糖与乙酸酐为原料,在微波辐射、无溶剂条件以及I2/IL400体系中,数分钟之内可以非常高的产率(90%–99%)和数十毫摩尔规模(50.0 mmol)制备出全乙酰糖.通过简单的甲苯萃取,可以从I2/IL400体系中分离出全乙酰糖,I2/IL400体系可循环使用6次,且产率均在90%以上.当反应规模扩大到50.0 mmol时,该体系依然能高效快速地催化糖的全乙酰化,并且可以循环使用5次,产率依然维持在90%左右.
A practical and highly efficient approach was developed to synthesize peracetylated sugar derivatives using a recyclable iodine/PEG_400-based ionic liquid catalyst(I_2/IL].The peracetylated sugars were readily obtained in a few minutes in excellent yields(90%-99%,13 examples]on a multi-gram scale(50.0 mmol) by the reaction of sugar and acetic anhydride under microwave irradiation in the absence of a volatile organic solvent.The desired product was easily obtained by simple extraction with toluene from the reaction mixture,and I_2/ILs can be readily recovered and reused at least six times without obvious loss in the yield.When the scale of the per-O-acetylation reaction was increased to 50.0 mmol,the desired product was still obtained in 90%yield after five recycles.