- Preparation method of 2-fluoroethylamine hydrochloride
-
The invention discloses a preparation method of 2-fluoroethylamine hydrochloride. The method comprises the following steps: S1, synthesis of 2-fluoroethyl phthalimide: adding 2-fluoro-1-haloethane and phthalimide potassium into a reaction container, performing dissolving with N,N-dimethylformamide under mechanical stirring, performing reacting, carrying out reduced pressure distillation to recover N,N-dimethylformamide after the reaction is finished, adding water into the reaction container, performing heating and stirring, and performing cooling, filtering and vacuum drying to obtain a 2-fluoroethyl phthalimide intermediate; and S2, synthesis of the 2-fluoroethylamine hydrochloride: adding the 2-fluoroethyl phthalimide intermediate prepared in the step S1 into the reaction container, performing dissolving with ethanol, dropwise adding hydrazine hydrate for reaction, performing cooling after the reaction is finished, adjusting the pH to 5 with hydrochloric acid, performing refluxing for 1 hour, and performing filtering and vacuum drying to obtain white flaky crystal 2-fluoroethylamine hydrochloride. The method is simple in process, green, safe, low in cost and high in yield.
- -
-
Paragraph 0021-0023; 0025-0026; 0028-0029
(2021/04/14)
-
- Preparation method of fluorine-containing primary amine intermediate
-
The invention discloses a preparation method of a fluorine-containing primary amine intermediate. The method comprises the following steps: directly fluorinating an N-hydroxyalkyl phthalimide compound serving as a raw material under the action of an organic solvent and a Lewis acid catalyst to obtain an N-fluoroalkyl phthalimide intermediate, and reducing the intermediate to obtain the fluorine-containing primary amine. According to the method, the raw materials are cheap and easy to obtain, the process route is simple and easy to control, the N-hydroxyalkylphthalimide can be effectively promoted to generate the corresponding fluoride at a high conversion rate, meanwhile, the dehydrofluorination reaction in the fluorination process can be avoided, the yield of the fluoride intermediate is 85% or above, the purity reaches 97% or above, and the method is suitable for large-scale production.
- -
-
Paragraph 0030-0031; 0032-0034; 0058
(2021/07/01)
-
- Deoxyfluorination of alcohols with aryl fluorosulfonates
-
Aryl fluorosulfonates are developed as a deoxyfluorinating reagent in the transformation of primary and secondary alcohols into the corresponding alkyl fluorides. These reagents feature easy availability, low-cost, high stability and high efficiency. Diverse functionalities including aldehyde, ketone, ester, halogen, nitro, alkene, and alkyne are well tolerated under mild reaction conditions.
- Fei, Zhongbo,Hu, Jinbo,Li, Wei,Liu, Qinghe,Ni, Chuanfa,Wang, Xiu,Zhou, Min
-
supporting information
p. 8170 - 8173
(2021/08/23)
-
- Transition-metal-free visible-light photoredox catalysis at room-temperature for decarboxylative fluorination of aliphatic carboxylic acids by organic dyes
-
We report herein an efficient, general and green method for decarboxylative fluorination of aliphatic carboxylic acids. By using a transition-metal-free, organocatalytic photoredox system, the reaction of various aliphatic carboxylic acids with the Select
- Wu, Xinxin,Meng, Chunna,Yuan, Xiaoqian,Jia, Xiaotong,Qian, Xuhong,Ye, Jinxing
-
supporting information
p. 11864 - 11867
(2015/07/20)
-
- Silver-catalyzed decarboxylative fluorination of aliphatic carboxylic acids in aqueous solution
-
Although fluorinated compounds have found widespread applications in the chemical and materials industries, general and site-specific C(sp3)-F bond formations are still a challenging task. We report here that with the catalysis of AgNO3, various aliphatic carboxylic acids undergo efficient decarboxylative fluorination with SELECTFLUOR reagent in aqueous solution, leading to the synthesis of the corresponding alkyl fluorides in satisfactory yields under mild conditions. This radical fluorination method is not only efficient and general but also chemoselective and functional-group- compatible, thus making it highly practical in the synthesis of fluorinated molecules. A mechanism involvinig Ag(III)-mediated single electron transfer followed by fluorine atom transfer is proposed for this catalytic fluorodecarboxylation.
- Yin, Feng,Wang, Zhentao,Li, Zhaodong,Li, Chaozhong
-
supporting information; experimental part
p. 10401 - 10404
(2012/08/08)
-
- Synthesis of N-(2-[18F]fluoroethyl)-N'-methylthiourea: A hydrogen peroxide scavenger
-
N-(2-[18F]fluoroethyl)-N'-methylthiourea ([18F]FEMTU), a fluorine- 18 labelled derivative of the hydrogen peroxide scavenger dimethylthiourea (DMTU), has been synthesized by reaction of 2-[18F]fluoroethylamine with methyli
- Gilissen,Bormans,De Groot,Verbruggen
-
p. 491 - 502
(2007/10/03)
-