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用Marvel的方法合成双端β-氯烯醛四苯醚砜(简称I_b)时生成大量的,不易回收的季铵盐混合液。合成双端炔基四苯醚砜(简称I)时,DMF溶剂的用量较大,有一定毒性。回收时损失25％以上,产品价格难免偏高,废液污染较严重,推广应用受到限制。针对以上问题,在合成反应过程中,对试剂和溶剂的用量,作了认真的考查。用红外、核磁等对产品进行了分析验证。在保证产品质量的情况下,达到了降低成本、提高经济效益的目的。
The synthesis of double-ended β-chloroaldehyde tetraphenyl ether sulfone (abbreviated as I_b) by Marvel’s method generates a large amount of quaternary ammonium salt mixture which is not easy to be recovered. Synthetic double-terminal alkynyl four ether sulfone (referred to as I), the larger the amount of DMF solvent, there is a certain toxicity. Recycling loss of more than 25%, the product will inevitably high prices, waste more serious pollution, promote the use of restricted. In view of the above problems, in the synthesis reaction process, the amount of reagents and solvents, made a careful examination. Using infrared, NMR and other products were analyzed and verified. In the case of ensuring product quality, reached the purpose of reducing costs and improve economic efficiency.