摘要
以D-甘露醇为原料,经丙叉基保护、氧化还原、苄基保护、脱丙叉保护、醇的酰化、苄基的脱保护合成了1,2-甘油二酯,中间体和目标产物结构经过了IR和元素分析鉴定。考察了不同的萃取溶剂和相转移催化剂对重要中间体甘油醇缩丙酮合成的影响。最终采用价廉的、环境友好的乙酸乙酯作为萃取溶剂,相转移催化剂季铵盐四丁基硫酸氢铵的质量分数为0.1%时效果最佳,并选择了"一锅法"合成的路线。考察了缚酸剂对中间体3-氧-苄基甘油合成的影响。在最优条件下,实验选择有机碱三乙胺作为3-氧-苄基甘油合成的缚酸剂。最终1,2-甘油二酯产率达到49.3%。
1,2-Diacylglycerol is synthesized by isopropylidene acetalformation, oxidation, benzylation, deprotection, acylation of alcohols and benzyl deprotection with D-mannitol as raw material. The chemical structures of intermediate and targeted product are characterized by IR and elemental analysis. The results are consistent with the molecular structures. The effects of extraction solvent and the phase transfer catalyst on the synthesis of the important intermediates 2,3-isopropylidene-sn-glycerol are investigated. The inexpensive, environmentally and friendly ethyl acetate is used as the extraction solvent. The optimal amount of phase transfer catalyst quaternary ammonium tetrabutyl ammonium hydrogen sulfate is 0. 1%. The ＂one pot＂ synthesis route is selected. The effect of acid binding agent on the synthesis of 3-o-benzyl glycerol is also investigated. Under the optimized conditions, the final yield of 1,2-diacylglycerol is 49. 3% with triethylamine as the acid binding agent.
出处
《现代化工》
CAS
CSCD
北大核心
2013年第1期73-75,77,共4页
Modern Chemical Industry
关键词
D-甘露醇
1
2-甘油二酯
相转移催化剂
缚酸剂
合成
D-mannitol
1,2-diacylglycerol
phase transfer catalyst
acid binding agent
synthesis
