Category: 20154-03-4

20154-03-4, name is 3-(Trifluoromethyl)-1H-pyrazole, belongs to pyrazoles-derivatives compound, is considered to be a conventional heterocyclic compound, which is widely used in drug synthesis. The chemical synthesis route is as follows. Safety of 3-(Trifluoromethyl)-1H-pyrazole

1,4-Diazabicyclo[2.2.2]octane (5.44 g, 48.5 mmol) and dimethylsulfamoyl chloride (4.76 mL, 44.46 mmol) were added to a solution of 3-(trifluoromethyl)pyrazole (5.5 g, 40.42 mmol) in acetonitrile (50 mL) at 0¡ã C. The mixture was allowed to warm to room temperature and stirred for 18 hours. The mixture was concentrated in vacuo and the residue was diluted with water. The product was extracted with AcOEt. The organic layer was separated, dried (MgSO4), filtered and the solvents evaporated in vacuo. The crude product was purified by flash column chromatography (silica gel; DCM). The desired fractions were collected and concentrated in vacuo to yield intermediate 43 (9.4 g, 95percent yield) as a colourless oil.

The synthetic route of 20154-03-4 has been constantly updated, and we look forward to future research findings.

Each compound has different characteristics, and only by selecting the characteristics of the compound suitable for a specific situation can the compound be applied on a large scale. 20154-03-4, name is 3-(Trifluoromethyl)-1H-pyrazole, This compound has unique chemical properties. The synthetic route is as follows., category: pyrazoles-derivatives

Step c: NaH (33.08 g (19.85, 60percent), 1.5 eq) was washed with hexane, dry DMF (500 ml) was added drop wise under N2 atmosphere and stirred well. A solution of 3-(trifluoromethyl)- 1 H-pyrazole (75 g, 550 mmol) in DMF (125 ml) was added drop wise under N2 atmosphere. Then a solution of 4-methoxylbenzyl chloride (86.3 g, 550 mmol, 1 eq) in DMF (125 ml) was added drop wise and the overall reaction mixture was allowed to stir for 12 h at room temperature. On completion of the reaction, reaction contents were poured into ice water (500 ml) and the product was extracted with ethyl acetate (2 * 400 ml). The ethyl acetate layer was washed with 2N HCI (2x200ml). Then the contents were dried over sodium sulfate and concentrated under reduced pressure. Obtained crude was purified by silica gel column chromatography with 10percent ethyl acetate/Hexane to yield the required product as a brown colored liquid (98 g, 70percent yield).

According to the analysis of related databases, 20154-03-4, the application of this compound in the production field has become more and more popular.

Synthetic Route of 20154-03-4, These common heterocyclic compound, 20154-03-4, name is 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.

NaH (33.08 g (19.85, 60percent), 1.5 equiv.) was added to a small amount of n-hexane and the mixture was stirred for 10 minutes. The n-hexane was decanted, dry DMF (500 mL) was added under an N2 atmosphere and the mixture was stirred. A solution of the product obtained in step b (75 g, 550 mmol) in DMF (125 mL) was added dropwise under an N2 atmosphere. A solution of 4-methoxyl benzoyl chloride (86.3 g, 550 mmol, 1 equiv.) in DMF (125 mL) was then added dropwise and the mixture was stirred for 12 h at RT and then poured into iced water (500 mL), and the mixture was extracted with EA (2.x.400 mL). The mixture was then dried over Na2SO4 and concentrated under reduced pressure, the crude product being obtained as a brown oil (125 g, 88percent yield).

Statistics shows that 3-(Trifluoromethyl)-1H-pyrazole is playing an increasingly important role. we look forward to future research findings about 20154-03-4.

Adding a certain compound to certain chemical reactions, such as: 20154-03-4, name is 3-(Trifluoromethyl)-1H-pyrazole, belongs to pyrazoles-derivatives compound, can increase the reaction rate and produce products with better performance than those obtained under traditional synthetic methods. Here is a downstream synthesis route of the compound 20154-03-4, Recommanded Product: 3-(Trifluoromethyl)-1H-pyrazole

Reference Production Example 12-1 4-bromo-3-(trifluoromethyl)-1H-pyrazole 3.50 g of 3-(trifluoromethyl)-1H-pyrazole was suspended in 45 ml of water, and 3.2 g of 50 % aqueous solution of sodium hydroxide was added to it. The mixture was cooled to 0 C, and then 3.20 g of bromine was added to the mixture, followed by stirring at room temperature for 7 hours. The reaction mixture was extracted by ethyl acetate. The organic layer was washed with water dried over anhydrous magnesium sulfate, filtered, and concentrated under reduced pressure. Hexane was added to the residue, as a result, a crystal was formed. The crystal was collected to obtain 3.38 g of 4-bromo-3-(trifluoromethyl)-1H-pyrazole. 1H-NMR(CDCl3,TMS,delta(ppm)):7.72(1H,s)

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Reference of 20154-03-4, A common heterocyclic compound, 20154-03-4, name is 3-(Trifluoromethyl)-1H-pyrazole, molecular formula is C4H3F3N2, 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.

From the indications on page 343 of Ref. refPreviewPlaceHolder49, the following procedure was designed: 3-(trifluoromethyl)-1H-pyrazolerefPreviewPlaceHolder [32] , refPreviewPlaceHolder33 M.E.F. Braibante, G. Clar, M.A.P. Martins and C. Jackson. J. Heterocycl. Chem., 30 (1993), pp. 1159-1160. [33] and refPreviewPlaceHolder[34] (1e) (5.54 g, 40.7 mol) and N-chlorosuccinimide (5.97 g, 44.7 mmol) in acetonitrile (13 mL) were heated in a microwave oven at 120 ¡ãC for 1 h. The resulting mixture was concentrated to dryness and dispersed in water (300 mL). The precipitate was filtered, rinsed with water and left to dry over 3 days to yield compound 3i (5.08 g, 73percent) as a powder; mp 94 ¡ãC 1H NMR (CDCl3): 7.69 (s, 1H); 11.2 (s (br), 1H). 13C NMR (CDCl3): 109.6; 120.2 (q, J=267 Hz); 129.5; 130.0 (q, J=37 Hz). HRMS: calcd for C4H2ClF3N2-H: 168.9780; Found: 168.9747.

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.

Electric Literature of 20154-03-4,Some common heterocyclic compound, 20154-03-4, name is 3-(Trifluoromethyl)-1H-pyrazole, molecular formula is C4H3F3N2, 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.

Step 1: Preparation of 1-(4-nitro-ph 1H-pyrazole1 -fluoro-4-nitro benzene (4.14 g, 29.4 mmol) was added slowly to a solution of 3- trifluoromethylpyrazole (2 g, 14.7 mmol) and anhydrous potassium carbonate (6 g, 44.1 mmol) in D F at room temperature.The reaction mixture was then heated at 110C overnight then cooled to RT. The reaction mixture was diluted with water then extracted with ethyl acetate (2 x). The combined organic layers were washed with water and brine, then dried over sodium sulfate, filtered and concentrated to give the title compound as a beige solid (3.3 g, 87.4%). TLC: Ethylacetate/Hexane (3/7): Rf : 0.85. 1H N R (CDCI3; 400 MHz): delta 8.38 (dd, J = 9.1 Hz, 2H), 8.10 (d, J = 2.4 Hz, 1 H), 7.94 (dd, J = 9.1 Hz, 2H), 6.83 (d, J = 2.5 Hz, 1 H).

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 3-(Trifluoromethyl)-1H-pyrazole, its application will become more common.

Adding a certain compound to certain chemical reactions, such as: 20154-03-4, name is 3-(Trifluoromethyl)-1H-pyrazole, belongs to pyrazoles-derivatives compound, can increase the reaction rate and produce products with better performance than those obtained under traditional synthetic methods. Here is a downstream synthesis route of the compound 20154-03-4, 20154-03-4

An acetonitrile solution (20 ml) of 3-trifluoromethyl-lH-pyrazole (0.5 g), dicerium ammonium nitrate (1.0 g) and N-chlorosuccinimide (0.7 g) was refluxed for 3 hours. After cooling, the reaction solution was washed with saturated aqueous solution of sodium thiosulfate and saturated aqueous solution of sodium chloride. After drying an organic layer with magnesium sulfate, the solvent was distilled off under the reduced pressure to obtain 4-chloro-3-trifluoromethyl-lH-pyrazole (0.9 g). ‘H-NMR (CDCl3, ppm): 7.80 (1H, s).

In the field of chemistry, the synthetic routes of compounds are constantly being developed and updated. I will also mention this compound in other articles, 3-(Trifluoromethyl)-1H-pyrazole, other downstream synthetic routes, hurry up and to see.

20154-03-4, 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 20154-03-4 as follows.

Example 104: Preparation of (S)-3-methyl-2-(8-(3-(trifluoromethyl)-lH- pyrazol-l-yl)dibenzo[b,d]furan-3-sulfonamido)butanoic acidStep 1 : Preparation of (SWert-butyl 3-methyl-2-(8-(3-(trifluoromethvO-lH-pyrazol- l-yDdibenzo[b,d1furan-3-ylsulfonamido)butanoate[0234] (S)-Tert-butyl 2-(8-bromodibenzo[b,d]furan-3-sulfonamido)-3- methylbutanoate from (Example 103, Step 2, 485 mg, 1 mmol), 3- (trifluoromethyl)pyrazole (274 mg, 2 mmol), /roem’-N,N’-dimethyl-l,2- cyclohexanediamine (29 mg, 0.2 mmol), copper (I) iodide (CuI, 10 mg, 0.05 mmol), and K3PO4 (450 mg, 21 mmol) were mixed in 2 mL of toluene. The mixture was irradiated with microwave at 13O0C for 3 hours. The reaction mixture was purified by a preparative etaPLC to give 313 mg of (S)-/erf-butyl 3-methyl-2-(8-(3- (trifluoromethyl)-l/7-pyrazol-l-yl)dibenzo[b,d]furan-3-ylsulfonamido)butanoate as a white solid in 58percent yield.

According to the analysis of related databases, 3-(Trifluoromethyl)-1H-pyrazole, the application of this compound in the production field has become more and more popular.

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 20154-03-4 as follows. 20154-03-4

EXAMPLE 7 (5,11-Dihydro-pyrido[2,3-b][1,5]benzodiazepin-6-yl)-[2-trifluoromethyl-4-(3-trifluoromethyl-pyrazol-1-yl)-phenyl]-methanone Sodium hydride (60percent suspension in oil, 0.17 g, 4.25 mmol) was washed with hexane, dried under nitrogen and resuspended in dry dimethylformamide (10 mL). 3-trifluoromethyl pyrazole (0.34 g, 2.5 mmol) was added in one portion. After the gas evolution subsided stirring was continued at room temperature. The (5,11-dihydro-pyrido [2,3-b][1,5]benzodiazepin-6-yl)- (4-fluoro-2-trifluoromethyl-phenyl)methanone of Example 4, Step B (0.75 g, 1.94 mmol) was added in one portion and the mixture was placed in an oil bath (preheated at 130¡ã C.) overnight. After cooling, the mixture was partitioned between water and ethyl acetate. The organic extracts were dried over sodium sulfate, and evaporated to dryness in vacuo. The residue was crystallized from ethanol to yield the title compound (0.57 g, 57.3percent) as an off-white solid, m.p. 127-129¡ã C. NMR (DMSO-d6, 400 MHz): delta 4.19 and 5.46 (dd, 2H, CONCH2), 6.54 (m, 1H), 6.70 (m, 1H), 6.80 (m, 1H), 7.02 (m, 1H), 7.07 (m, 1H, pyrazole CH), 7.29 (m, 1H), 7.61 (m, 1H), 8.00 (m, 1H), 8.05-8.16 (m, 2H), 8.84 (m, 1H, pyrazole CH), 9.63 (s, 1H, NH) MS (EI, m/z): 503 [M]+ Anal. Calc’d for C24 H15 F6 N5 O: C 57.26, H 3.00, N 13.91. Found: C 57.07, H 2.97, N 13.58

According to the analysis of related databases, 20154-03-4, the application of this compound in the production field has become more and more popular.