Category: 19968-17-3

These common heterocyclic compound, 19968-17-3, name is 4-Bromo-3-(trifluoromethyl)-1H-pyrazole, its traditional synthetic route has been very mature, but the traditional synthetic route has various shortcomings, such as complicated route, low yield, poor purity, etc, below Introduce a new synthetic route. Recommanded Product: 4-Bromo-3-(trifluoromethyl)-1H-pyrazole

3-Methyl-4-nitrobenzyl chloride (0.77 g), 4-bromo-3-trifluoromethyl-lH-pyrazole (0.90 g) and po- tassium carbonate (0.57 g) were stirred in DMF (10 ml) at room temperature for 2 hours. The reaction solution was diluted with ethyl acetate and washed with water and saturated aqueous solution of so- dium chloride. After drying the organic layer with magnesium sulfate, the solvent was distilled off under the reduced pressure and the obtained residue was purified by silica gel column chromatogra- phy to obtain 1- (3-methyl-4-nitrobenzyl)-4-bromo-3-trifluoromethyl-lH-pyrazole (0.9 g). ‘H-NMR (CDCl3, ppm): 2.58 (3H, s), 5.35 (2H, s), 7.24-7. 21 (2H, m), 7.49 (1H, s), 7. 98 (1H, d).

The synthetic route of 4-Bromo-3-(trifluoromethyl)-1H-pyrazole has been constantly updated, and we look forward to future research findings.

Reference:
Patent; BAYER CROPSCIENCE AG; WO2005/95351; (2005); A1;,
Pyrazole – Wikipedia,
Pyrazoles – an overview | ScienceDirect Topics

Electric Literature of 19968-17-3, In the chemical reaction process, reaction time, type of solvent, can easily affect the result of the reaction, thereby determining the yield and properties of the reaction product. An updated downstream synthesis route of 19968-17-3 as follows.

To a solution of 4-bromo-3-trifluoromethyl-lH-pyrazole 33 (0.645 g, 3 mmol) in dimethylformamide (DMF) (50 niL) was added NaH (0.2 g, 9 mmol). The mixture was stirred for 0.5 h at room temperature and the 2-bromo-l ,3-thiazole (0.76 g, 4.5 mmol) was added. The reaction mixture was stirred for 1 h at room temperature. The reaction temperature was raised to 90C and stirred for overnight. The reaction was quenched with MeOH and solvent was removed in vacuo. The residue was treated with water and EtOAc. The organic layer was separated and aqueous was extracted with EtOAc. The combined organic phase was dried over Na2S04, filtered, and concentrated to give crude product. The crude product was purified on ISCO columns. Fractions containing pure product were combined and evaporated to give 34 as a brown oil (0.45 g, 50%).

According to the analysis of related databases, 19968-17-3, the application of this compound in the production field has become more and more popular.

Reference:
Patent; CALCIMEDICA, INC.; WHITTEN, Jeffrey, P.; CAO, Jianguo; WANG, Zhijun; GREY, Jonathan; ROGERS, Evan; WO2015/54283; (2015); A1;,
Pyrazole – Wikipedia,
Pyrazoles – 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. 19968-17-3, name is 4-Bromo-3-(trifluoromethyl)-1H-pyrazole, A new synthetic method of this compound is introduced below., HPLC of Formula: C4H2BrF3N2

4-Bromo-1-{[(4R)-2,2-dimethyl-1,3-dioxolan-4-yl]methyl}-5-(trifluoromethyl)-1H-pyrazole and 4-bromo-1-{[(4R)-2,2-dimethyl-1,3-dioxolan-4-yl]methyl}-3-(trifluoromethyl)-1H-pyrazole; A mixture of 4-bromo-3-trifluoromethyl-1H-pyrazole (400.0 mg, 1.861 mmol), toluene-4-sulfonic acid (S)-2,2-dimethyl-[1,3]dioxolan-4-ylmethyl ester (799.2 mg, 2.791 mmol), K2CO3 (400.0 mg, 2.894 mmol) and DMF (6 mL, 80 mmol) was heated to 90 C. for 2 h. The material was extracted with EtOAc, washing with water (3¡Á). The organic layer was dry-loaded onto silica gel, and purified via column chromatography, eluting with 10-30% EtOAc/heptane. The fractions containing each pure product were concentrated in vacuo to afford the title compounds as clear oils. 3-Trifluoromethyl isomer: 1H NMR (400 MHz, CD3OD): delta=1.31 (s, 3H), 1.34 (s, 3H), 3.78 (dd, J=8.6, 5.8 Hz, 1H), 4.10 (dd, J=8.8, 6.6 Hz, 1H), 4.22-4.31 (m, 1H), 4.36 (dd, J=14.1, 4.0 Hz, 1H), 4.41-4.49 (m, 1H), 7.92 (s, 1H). MS (ES+): m/z=329.01/331.01 (100/100) [MH+]. HPLC: tR=1.59 min (polar-3 min, UPLC-ACQUITY). 5-Trifluoromethyl isomer: MS (ES+): m/z=329.01/331.01 (100/100) [MH+]. HPLC: tR=1.62 min (polar-3 min, UPLC-ACQUITY).

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.

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. 19968-17-3, name is 4-Bromo-3-(trifluoromethyl)-1H-pyrazole, A new synthetic method of this compound is introduced below., COA of Formula: C4H2BrF3N2

To a solution of 4-bromo-3- (trifluoromethyl) -1H-pyrazole (1.01 g, 4.7 mmol) in DMF (40 mL)2- (bromineMethyl) pyridine hydrobromide (1.76 g, 6.96 mmol), Cs2CO3 (5.3 g, 16 mmol) and KI (0.4 g, 2 mmol)100 for 10h. The reaction mixture was concentrated under reduced pressure to remove DMF, extracted with water (40 mL) and extracted with methylene chloride (50 mL ¡Á 3), and then the organicThe phases were dried over anhydrous Na2SO4. The concentrated crude product was isolated by silica gel column chromatography (eluent: PE / EtOAc (v / v) = 1 /1) to give 1.2 g of a yellow oil, yield: 83%.

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.