目的研究牛磺酸的合成新工艺。方法以乙醇胺(MEA)为原料,在改性HZSM-5分子筛催化剂作用下,经分子内脱水和与亚硫酸氢胺开环加成两步反应制备牛磺酸。结果分子内脱水的适宜工艺条件是:反应温度为425℃、反应压力为常压、反应器空速为2 30...目的研究牛磺酸的合成新工艺。方法以乙醇胺(MEA)为原料,在改性HZSM-5分子筛催化剂作用下,经分子内脱水和与亚硫酸氢胺开环加成两步反应制备牛磺酸。结果分子内脱水的适宜工艺条件是:反应温度为425℃、反应压力为常压、反应器空速为2 300 h 1、反应原料配比为N2/MEA=10。在该条件下,乙醇胺的转化率93.2%,选择性84.6%,牛磺酸的总收率为73%(以乙醇胺计)。结论新工艺优于乙醇胺酯化法(>50%)和环氧乙烷法(>60%),具有很好的工业化前景。展开更多
目的合成一系列脂酰苯丙氨酸凝胶因子——肉豆蔻酰-苯丙氨酸甲酯（C14-L-Phe-OMe）、棕榈酰-苯丙氨酸甲酯（C16-L-Phe-OMe）及硬脂酰-苯丙氨酸甲酯（C18-L-Phe-OMe）,并对其进行结构表征和性质考察。方法以L-苯丙氨酸甲酯盐酸盐为母核,...目的合成一系列脂酰苯丙氨酸凝胶因子——肉豆蔻酰-苯丙氨酸甲酯（C14-L-Phe-OMe）、棕榈酰-苯丙氨酸甲酯（C16-L-Phe-OMe）及硬脂酰-苯丙氨酸甲酯（C18-L-Phe-OMe）,并对其进行结构表征和性质考察。方法以L-苯丙氨酸甲酯盐酸盐为母核,肉豆蔻酰氯、棕榈酰氯、硬脂酰氯为酰化剂,合成一系列脂酰苯丙氨酸凝胶因子,采用IR、1H-NMR、MS等手段对其结构进行表征,并考察其熔点、一级大豆油中的相转变温度和凝胶能力。结果成功合成了C14-L-Phe-OMe、C16-L-Phe-OMe及C18-L-Phe-OMe,并确证了其结构;三种凝胶因子的熔程分别为61.3~63.1、72.1~73.0和62.3~64.1;胶凝能力大小顺序是：C16-L-Phe-OMe〉C18-L-Phe-OMe〉C14-L-Phe-OMe;三种凝胶因子在一级大豆油中的胶凝焓变分别为42.58 k J/mol、22.61 k J/mol和65.01 k J/mol。结论合成的一系列脂酰苯丙氨酸凝胶因子具有较好的胶凝能力,其中C16-L-Phe-OMe的胶凝能力最强,有望作为一种局部给药的长效释药载体。展开更多
We have synthesized mannich base cyclohexanone using microwave irradiation method,and studied their pharma-cological activity.Based on analytical and spectral(IR,NMR and Mass) data,a number of mono as well as double m...We have synthesized mannich base cyclohexanone using microwave irradiation method,and studied their pharma-cological activity.Based on analytical and spectral(IR,NMR and Mass) data,a number of mono as well as double mannich base cyclohexanones have been synthesized from primary and secondary amines and formaldehyde,and then purified and characterized. The required 3-aryl-2,4-diacetyl-5-hydroxy-5-methylcyclohexanone was prepared from appropriate aldehyde and acetylacetone. The synthesized compounds were screened for analgesic activity via standard approaches,and they have shown positive analgesic activity.展开更多
Kdo residues are widely distributed in bacteria.They are components of bacterial lipopolysaccharide(LPS)and capsular polysaccharides,which can be recognized by the human adaptive immune system,and have great potential...Kdo residues are widely distributed in bacteria.They are components of bacterial lipopolysaccharide(LPS)and capsular polysaccharides,which can be recognized by the human adaptive immune system,and have great potential for developing new sugar chips and antibacterial vaccines.By improving the existing methods,we optimized the Kdo chemical synthesis method,which was able to efficiently synthesize Kdo monosaccharides with high purity,laying a foundation for the construction of subsequent compound libraries.Kdo acylation can easily form 1,5-lactones and reduce the efficiency of synthesis.By changing the synthesis sequence,we avoided the formation of Kdo 1,5-lactones,improved the synthesis efficiency of Kdo glycals,and provided a new strategy for derivatization.展开更多
Two total synthetic routes for the preparation of myricetin were designed and explored.It was validated that route B presented an efficient approach to synthesizing myricetin,starting from commercially available and i...Two total synthetic routes for the preparation of myricetin were designed and explored.It was validated that route B presented an efficient approach to synthesizing myricetin,starting from commercially available and inexpensive phloroglucinol.Myricetin was synthesized with an overall yield of 60%across three steps without the need of column chromatography separation.The successful preparation of myricetin on a 25-g scale underscored the potential of this approach.展开更多
文摘目的研究牛磺酸的合成新工艺。方法以乙醇胺(MEA)为原料,在改性HZSM-5分子筛催化剂作用下,经分子内脱水和与亚硫酸氢胺开环加成两步反应制备牛磺酸。结果分子内脱水的适宜工艺条件是:反应温度为425℃、反应压力为常压、反应器空速为2 300 h 1、反应原料配比为N2/MEA=10。在该条件下,乙醇胺的转化率93.2%,选择性84.6%,牛磺酸的总收率为73%(以乙醇胺计)。结论新工艺优于乙醇胺酯化法(>50%)和环氧乙烷法(>60%),具有很好的工业化前景。
文摘目的合成一系列脂酰苯丙氨酸凝胶因子——肉豆蔻酰-苯丙氨酸甲酯（C14-L-Phe-OMe）、棕榈酰-苯丙氨酸甲酯（C16-L-Phe-OMe）及硬脂酰-苯丙氨酸甲酯（C18-L-Phe-OMe）,并对其进行结构表征和性质考察。方法以L-苯丙氨酸甲酯盐酸盐为母核,肉豆蔻酰氯、棕榈酰氯、硬脂酰氯为酰化剂,合成一系列脂酰苯丙氨酸凝胶因子,采用IR、1H-NMR、MS等手段对其结构进行表征,并考察其熔点、一级大豆油中的相转变温度和凝胶能力。结果成功合成了C14-L-Phe-OMe、C16-L-Phe-OMe及C18-L-Phe-OMe,并确证了其结构;三种凝胶因子的熔程分别为61.3~63.1、72.1~73.0和62.3~64.1;胶凝能力大小顺序是：C16-L-Phe-OMe〉C18-L-Phe-OMe〉C14-L-Phe-OMe;三种凝胶因子在一级大豆油中的胶凝焓变分别为42.58 k J/mol、22.61 k J/mol和65.01 k J/mol。结论合成的一系列脂酰苯丙氨酸凝胶因子具有较好的胶凝能力,其中C16-L-Phe-OMe的胶凝能力最强,有望作为一种局部给药的长效释药载体。
文摘We have synthesized mannich base cyclohexanone using microwave irradiation method,and studied their pharma-cological activity.Based on analytical and spectral(IR,NMR and Mass) data,a number of mono as well as double mannich base cyclohexanones have been synthesized from primary and secondary amines and formaldehyde,and then purified and characterized. The required 3-aryl-2,4-diacetyl-5-hydroxy-5-methylcyclohexanone was prepared from appropriate aldehyde and acetylacetone. The synthesized compounds were screened for analgesic activity via standard approaches,and they have shown positive analgesic activity.
基金National Natural Science Foundation of China(Grant No.81930097,21977005)。
文摘Kdo residues are widely distributed in bacteria.They are components of bacterial lipopolysaccharide(LPS)and capsular polysaccharides,which can be recognized by the human adaptive immune system,and have great potential for developing new sugar chips and antibacterial vaccines.By improving the existing methods,we optimized the Kdo chemical synthesis method,which was able to efficiently synthesize Kdo monosaccharides with high purity,laying a foundation for the construction of subsequent compound libraries.Kdo acylation can easily form 1,5-lactones and reduce the efficiency of synthesis.By changing the synthesis sequence,we avoided the formation of Kdo 1,5-lactones,improved the synthesis efficiency of Kdo glycals,and provided a new strategy for derivatization.
基金The Clinical Medicine Special Project of Nantong University for financial support(Grant No.2022JQ011)。
文摘Two total synthetic routes for the preparation of myricetin were designed and explored.It was validated that route B presented an efficient approach to synthesizing myricetin,starting from commercially available and inexpensive phloroglucinol.Myricetin was synthesized with an overall yield of 60%across three steps without the need of column chromatography separation.The successful preparation of myricetin on a 25-g scale underscored the potential of this approach.
