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ChemicalBook CAS DataBase List Ethyl trifluoromethanesulfonate

Ethyl trifluoromethanesulfonate synthesis

11synthesis methods
Triethyl orthoformate (4.44g,30mmol) was slowly added to trifluoromethanesulfonic anhydride (8.47g,30mmol) under ice bath, transferred to 25°C for reaction, monitored by NMR for 15 min, and the reaction was completed, distilled under reduced pressure to obtain 10.15g of ethyl trifluoromethanesulfonate colorless liquid in 94% yield.
-

Yield:425-75-2 92.7%

Reaction Conditions:

at 60 - 140;Large scale;Temperature;

Steps:

3
(1) 300g of trifluoromethanesulfonic acid and 154g of diethyl sulfate were put into a 5L glass reactor, stirring was started, then the reactor was heated to 60 ° C and incubated for 2 hours. (2) The reactor was heated to 120 ~ 140 ° C, open the rectification valve, control reflux ratio of 3: 1; the same time, to the reactor by adding trifluoromethanesulfonic acid and diethyl sulfate, Sulfonic acid at a rate of 30g / min continuously added to the reactor, diethyl sulfate to 15g / min rate continuously added to the reactor, the reaction rectification, the rectification tower top temperature stable at 115 ± 3 ° C , The fractions were collected and condensed, and the purity of ethyl triflate was 99.4% in the distillate, and the product was transferred to a finished collecting tank. The trial put a total of trifluoromethanesulfonic acid 3Kg, diethyl sulfate 1. 54Kg, received the product ethyl trifluoromethanesulfonate 3. 32Kg, yield 92.7%.

References:

Zhangjiagang Guotai-Huarong New Chemical Materials Co., Ltd;Xu, Xiao Qiang;Li, Jian Zhong;Guo, Jun;Shi, suping;Qian, xiaobing;He, Yong Gang;Yu, sanbao;Yang, Sheng CN103880715, 2016, B Location in patent:Paragraph 0018; 0019

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