化学研究与应用
化學研究與應用
화학연구여응용
CHEMICAL RESEARCH AND APPLICATION
2015年
5期
629-634
,共6页
谢建勇%马欢%刘浩%李勤耕
謝建勇%馬歡%劉浩%李勤耕
사건용%마환%류호%리근경
维生素E%异植物醇%格氏反应%Carroll重排%合成
維生素E%異植物醇%格氏反應%Carroll重排%閤成
유생소E%이식물순%격씨반응%Carroll중배%합성
Vitamin E%isophytol%Grignard reaction%Carroll rearrangement%synthesis
以丙酮为起始原料,经过格氏反应、Carroll重排、氢化反应得到异植物醇,总收率69.4%。该工艺提高收率的关键步骤Carroll重排反应选用异丙醇铝为催化剂,并对反应机理进行了初步探讨。目标产物和关键中间体经MS谱,1 H-NMR谱等确证了结构。改进后的合成工艺路线生产设备简单,条件温和,收率高,适合大规模化生产。
以丙酮為起始原料,經過格氏反應、Carroll重排、氫化反應得到異植物醇,總收率69.4%。該工藝提高收率的關鍵步驟Carroll重排反應選用異丙醇鋁為催化劑,併對反應機理進行瞭初步探討。目標產物和關鍵中間體經MS譜,1 H-NMR譜等確證瞭結構。改進後的閤成工藝路線生產設備簡單,條件溫和,收率高,適閤大規模化生產。
이병동위기시원료,경과격씨반응、Carroll중배、경화반응득도이식물순,총수솔69.4%。해공예제고수솔적관건보취Carroll중배반응선용이병순려위최화제,병대반응궤리진행료초보탐토。목표산물화관건중간체경MS보,1 H-NMR보등학증료결구。개진후적합성공예로선생산설비간단,조건온화,수솔고,괄합대규모화생산。
The target compound was synthesized through Grignard reaction,Carroll rearrangement and hydrogenation reaction from acetone with an overall yield of 69. 4%. Carroll rearrangement,the key step to improve the yield,was catalyzed by aluminum iso-propoxide,and the corresponding reaction mechanism was investigated preliminarily. The target compound and key intermediates were confirmed by MS and 1 H-NMR. The improved synthesis was benefited from simple equipment,mild conditions,high yield and could be readily scale-up to mass production.