Category: 348-65-2

Application of 348-65-2, As we all know, there are many different methods for the synthesis of a compound, and people can choose the synthesis method that suits their own laboratory according to the actual situation. 348-65-2 name is 5-Chloro-2,4-difluoroaniline, This compound is widely used in many fields, so it is necessary to find a new synthetic route. The downstream synthesis method of this compound is introduced below.

In a 500 mL two-neck round-bottomed flask equipped with magnetic stirrer, 5-chloro-2,4-difluoroaniline (10 g,61 mmol, 1 eq) was dissolved in DCM (150 mL, HPLC grade). Then, prop-2-ynoic acid (5.5 g, 78 mmol, 1.3 eq) wasadded dropwise (the salt of the amine appeared). Next EDC·HCl (14 g, 78 mmol, 1.3 eq) was added in several portions(during the addition the reaction flask was cooled in an ice bath to maintain the room temperature. After full addition ofEDC·HCl, the reaction mixture was stirred for an additional 1 h at room temperature. After that time 150 ml of water wasadded and the mixture was transferred into a separatory funnel. The phases were separated. The water phase wasextracted twice with the DCM (2 x 100 mL). The organic fractions were combined, washed with brine, dried over MgSO4and concentrated to approximately 50 ml in vacuo, resulting a thick suspension. The solids were filtered and dried tofurnish 8 g of cream crystals. The filtrate was concentrated and then purified by flash chromatography (n-hexane/AcOEt;8:1 ? 5:1) giving additional 4.4 g of the amide C-6F. As a result, expected amide C-6F was obtained as a cream solid(12.4 g, 94 % yield, 100 % purity according to UPLCMS analysis).

At the same time, in my other blogs, there are other synthetic methods of this type of compound, 5-Chloro-2,4-difluoroaniline, and friends who are interested can also refer to it.

Reference:
Patent; Adamed sp. z o.o.; FEDER, Marcin; MAZUR, Maria; KALINOWSKA, Iwona; JASZCZEWSKA, Joanna; LEWANDOWSKI, Wojciech; WITKOWSKI, Jakub; JELEN, Sabina; WOS-LATOSI, Katarzyna; (56 pag.)EP3511334; (2019); A1;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Researchers who often do experiments know that organic synthesis is a process of preparing more complex target molecules from simple raw materials through one or more chemical reactions. Generally, it requires fewer steps, and cheap raw materials. 348-65-2, name is 5-Chloro-2,4-difluoroaniline, A new synthetic method of this compound is introduced below., Recommanded Product: 5-Chloro-2,4-difluoroaniline

j00283j A solution of 5-chloro-2,4-difluoro-aniline (5.0 g, 31 mmol) and potassium 0-ethyl carbonodithioate (12 g, 73 mmol) in 1V N-dimethylformamide (50 mL) was stirred at 130 C for 16hours. On completion, the reaction was cooled to room temperature, and iN hydrochloric acid (100 mL) was added. The mixture was stirred for 1 hour, resulting in formation of a solid. The solid was collected by filtration, washed with water (2×100 mL) and dried under vacuum to give compound B- 5(5.6 g, 79% yield) as a white solid. LCMS (B): tR=0.759 mi, (ES)m/z(M+H)=220.1.

The basis of chemical reaction formula synthesis, the synthesis route is composed of some specific reactions and combined according to certain logical thinking. We look forward to the emergence of more reaction modes in the future.

Reference:
Patent; FORUM PHARMACEUTICALS, INC.; ACHARYA, Raksha; BURNETT, Duane, A.; BURSAVICH, Matthew, Gregory; COOK, Andrew, Simon; HARRISON, Bryce, Alden; McRINER, Andrew, J.; (267 pag.)WO2017/69980; (2017); A1;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics