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以碳酸二甲酯和β-环糊精为原料,以无水碳酸钾为催化剂,在N,N-二甲基甲酰胺介质中,考察了常压和高压条件下温度在50~170℃碳酸二甲酯对β-环糊精的改性作用。所得产品用制备型高效液相色谱分离纯化,用红外光谱、质谱和核磁共振光谱进行了表征。结果表明,在50~85℃,发生的是低取代的甲氧羰基化反应;在90~140℃,甲氧羰基化和甲基化反应均有发生;在160~170℃,压力约为1.40 MPa时,主要反应产物为取代度为7~9的随意甲基化β-环糊精,且收率达80%~85%。
Taking dimethyl carbonate and β-cyclodextrin as raw materials and anhydrous potassium carbonate as catalyst in N, N-dimethyl formamide medium, the effects of temperature Modification of β - Cyclodextrin with Dimethyl. The resulting product was purified by preparative HPLC and characterized by IR, MS and NMR spectra. The results showed that the low-substituted methoxycarbonylation occurred at 50-85 ° C. Both methoxycarbonylation and methylation occurred at 90-140 ° C. At 160-170 ° C, the pressure was about 1.40 MPa, the main reaction product was random methylated β-cyclodextrin with the substitution degree of 7-9, and the yield was 80% -85%.