摘要
以氯甲烷(2)为原料制备甲基氯化镁格氏试剂;以三氯化镓为催化剂,甲基氯化镁与1,1,1-三氟丙酮(3)反应,经水解制得1,1,1-三氟-2-甲基-2-丙醇(1)。产物结构经^(1)H-NMR、^(13)C-NMR、^(19)F-NMR及MS表征;通过单因素、正交实验和放大重复性实验确定了最佳反应条件:溶剂为正丁醚、格氏试剂浓度3 mol·L^(-1)、n(Mg)∶n(2)为1.05∶1、n(2)∶n(3)为1.3∶1、n(三氯化镓)∶n(3)为5%、3滴加及反应温度-10℃、反应12 h,平均收率为91.8%。该法具有原料价廉,操作方便,收率高,对环境友好等优点,适合规模生产。
1,1,1-Trifluoro-2-methyl-2-propanol(1)was synthesized by 1,1,1-trifluoroacetone(3)and methylmagnesium chloride prepared with methyl chloride(2)and magnesium as the raw materials in n-dibutyl ether,in the presence of gallium trichloride as catalyst.The structure of the product was investigated by ^(1)H-NMR,^(13)C-NMR,^(19)F-NMR and MS.The optimal condition was confirmed by orthogonal experimental design and repeated magnify experiments.The average yield of 1 was 91.8%under the optimal reaction conditions[n(Mg)∶n(2)=1.05∶1,n(2)∶n(3)=1.3∶1,n(gallium trichloride)∶n(2)=5%,at-10℃for 12 h].The method improved was operation-convenient,environment-friendly and suitable for a scale production.
作者
赵爱明
倪秋洋
ZHAO Ai-ming;NI Qiu-yang(HaiMen RuiYi Medical Science and Technology Company,Haimen 226121,China;KaiMei Chemical Science and Technology(NanTong)Company,Nantong 226100,China)
出处
《化学研究与应用》
CAS
CSCD
北大核心
2022年第1期207-213,共7页
Chemical Research and Application
关键词
格氏试剂
氯甲烷
1
1
1-三氟丙酮
三氯化镓
正交实验
Grignard reagent
methyl chloride
1,1,1-trifluoroacetone
gallium trichloride
orthogonal experimental design
