公开(公告)号：US06939962B2

公开(公告)日：2005-09-06

申请号：US10343378

申请日：2001-07-19

申请人： Jason D. Clark ,  Richard R. LeMay, Jr.

发明人： Jason D. Clark ,  Richard R. LeMay, Jr.

IPC分类号： B01J31/12 ,  C07B61/00 ,  C07H13/02 ,  C07H13/04 ,  C07H13/06 ,  C07H1/00 ,  C07H15/04

CPC分类号： C07H13/04 ,  C07H13/06

摘要： 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.

摘要翻译： 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）在大约97℃和大约50kpa进行，直到当第一反应混合物中锡与水的重量比大于约26时，当锡含量通过X射线荧光分析仪 ，并用Karl-Fischer法测量含水量。