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    • 75. 发明公开
    • 수크로오스-6-에스테르의 개선된 합성방법
    • 一种改进的蔗糖-6酯合成方法
    • KR1020070094671A
    • 2007-09-20
    • KR1020077019987
    • 2001-07-19
    • 테이트 앤드 라일 퍼블릭 리미티드 컴파니
    • 클라크재이슨디.르메이리차드알.쥬니어
    • C07H13/04C07H13/00
    • C07H13/04C07H13/06
    • There is described a process for the synthesis of a sucrose-6-ester comprising: (a) reacting a mixture comprising sucrose and a polar aprotic solvent with an organotin-based acylation promoter, while adding a solvent capable of removing water by co-distillation, and removing water by co-distillation, to afford a first reaction mixture which is substantially free from water, followed by (b) adding a carboxylic anhydride to said first reaction mixture to afford a second reaction mixture, and maintaining said second reaction mixture at a temperature and for a period of time sufficient to produce a sucrose-6-ester, characterised in that step (a) is performed at a temperature of from 85 to 125 °C and at a pressure of from 20 to 80 kPa. In the most preferred embodiment, the polar aprotic solvent is DMF, the solvent capable of removing water by co-distillation is cyclohexane, the organotion-based acylation promoter is a 1,3-diacyloxy-1,1,3,3-tetrabutyldistannoxane, and step (a) is performed at approximately 97 °C, and approximately 50 kPa, until the weight ratio of tin to water in the first reaction mixture is greater than about 26, when the tin content is measured by X-Ray Fluoresence Analyzer, and the water content is measured by the Karl- Fischer method.
    • 描述了合成蔗糖-6-酯的方法,其包括:(a)使包含蔗糖和极性非质子溶剂的混合物与有机锡基酰化促进剂反应,同时加入能够通过共蒸馏除去水的溶剂 ,并通过共蒸馏除去水,得到基本上不含水的第一反应混合物,然后(b)向所述第一反应混合物中加入羧酸酐以提供第二反应混合物,并将所述第二反应混合物保持在 温度和足以产生蔗糖-6-酯的一段时间,其特征在于步骤(a)在85至125℃的温度和20至80kPa的压力下进行。 在最优选的实施方案中,极性非质子溶剂是DMF,通过共蒸馏除去水的溶剂是环己烷,基于有机物的酰化促进剂是1,3-二酰氧基-1,1,3,3-四丁基二锡氧烷, 并且步骤(a)在约97℃和约50kPa下进行,直到第一反应混合物中锡与水的重量比大于约26时,当用X射线荧光分析仪测量锡含量时, 并用Karl-Fischer法测量含水量。