ChemicalBook CAS DataBase List 3,3,3-Trifluoropropionic acid

3,3,3-Trifluoropropionic acid synthesis

12synthesis methods

Product Name:3,3,3-Trifluoropropionic acid
CAS Number:2516-99-6
Molecular formula:C3H3F3O2
Molecular Weight:128.05

3,3,3-Trifluoropropionic acid can be reduced to trifluoropropanal or trifluoropropanol by lithium aluminum hydride or sodium borohydride, or it can be reduced to trifluoropropanol by hydrogenation in the presence of Rh/C catalyst. The CF3 group of 3,

460-40-2
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2516-99-6
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Yield:2516-99-6 96.1%

Reaction Conditions:

with tetrabutoxytitanium;sodium molybdate;dihydrogen peroxide;calcium chloride in ethanol;water at 75 - 90; for 6 h;Inert atmosphere;Time;

Steps:

1; 2; 3; 4; 5; 6 Example 2 An efficient synthesis method of 3,3,3-trifluoropropionic acid, comprising the following steps
(1) The walnut shell is dried and crushed and steamed, and then immersed in a calcium chloride solution for 15 hours, taken out and dried, and sieved to obtain a walnut shell powder; wherein the ratio of the walnut shell powder and the calcium chloride solution is Is 1g: 50mL;(2) Stir and mix the walnut shell powder and absolute ethanol, then add tetrabutyl titanate, then pass the nitrogen with water, reflux at 150 ° C for 20 h, cool to room temperature after the reaction, filter, The precipitate was washed 3-5 times with deionized water and absolute ethanol, dried, and the obtained powder was mixed with sodium molybdate and sintered at 800-900 ° C for 3 h to obtain a catalyst; among them, walnut shell powder, no The ratio of water ethanol and tetrabutyl titanate is 1g: 100mL: 1.5mL; the mass ratio of powder and sodium molybdate is 4:1;(3) Add 3,3,3-trifluoropropanal and hydrogen peroxide to the reactor, stir and mix well, then add the catalyst prepared above, raise the temperature to 75-90 ° C, stir the reaction for 6 h, and cool to room temperature after the reaction is completed. , filtering, removing the catalyst, collecting the filtrate, using diethyl ether as an extracting agent, collecting the extracting phase, removing the extracting agent under normal pressure, and then distilling under reduced pressure to collect a fraction of 6 kPa/70-75 ° C to obtain a target product; wherein, hydrogen peroxide, 3, The mass ratio of 3,3-trifluoropropanal to the catalyst was 1:2:0.03.

References:

Jiaxing Xiuzhou Qu Hong Hezhen Middle School;Zhu Shengxiang CN109400462, 2019, A Location in patent:Paragraph 0021-0052

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