Category: 327-75-3

Reference of 327-75-3,Some common heterocyclic compound, 327-75-3, name is 1-Bromo-2,4-bis(trifluoromethyl)benzene, molecular formula is C8H3BrF6, 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.

To a stirred solution of 4-nitro-lH-pyrazole (2.0 g, 6.51 mmol, 1 eq) in DMF (20ml) was added K CO portion wise at 0 C and stirred for 10 minutes. l-(bromomethyl)-2,4- bis(trifluoromethyl)benzene (0.73 gm, 6.51 mmol, 1 eq) was added drop wise 0 C. The reaction mixture was allowed to stir for 1 hour at RT. Product formation was confirmed by LCMS. After completion of reaction, reaction mixture was diluted with water and extracted with ethyl acetate (100 mL X 3). Combined organic extracts were washed with water (100 mL x 4), dried over anhydrous Na2S04 and concentrated under reduced pressure to obtain 1- (2,4-bis (trifluoromethyl) benzyl)-4-nitro-lH-pyrazole (2.1 g, as white solid). LCMS: 326 [M+H]+.

The synthetic route of 327-75-3 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; PRAXIS BIOTECH LLC; ALFARO, Jennifer; BELMAR, Sebastian; NUNEZ VASQUEZ, Gonzalo Esteban; PUJALA, Brahmam; SATHE, Balaji Dashrath; BERNALES, Sebastian; CHAKRAVARTY, Sarvajit; THAKRAL, Pooja; PATIDAR, Rajesh Kumar; (344 pag.)WO2019/195810; (2019); A2;,
Bromide – Wikipedia,
bromide – Wiktionary

Reference of 327-75-3, A common heterocyclic compound, 327-75-3, name is 1-Bromo-2,4-bis(trifluoromethyl)benzene, molecular formula is C8H3BrF6, 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.

Intermediate 33. 2-(2,4-Bis-trifluoromethyl-phenoxy)-ethylamine. [00136] Step A:; (2-Hydroxy-ethyl) -carbamic acid tert-butyl ester (0.2 mL, 1.29 mmol) is dissolved in 3 mL dry dimethyl-acetamide. 2-Potassium-1,1,1,3,3,3-hexamethyl- disilazane (0.52 g, 2.6 mmol, 2 equiv. ) is added, followed by 1-bromo-2,4-bis- trifluoromethyl-benzene 31 (0.26 mL, 1.5 mmol, 1.2 equiv. ). The mixture is stirred at 60C under nitrogen for 18 hours. The mixture is cooled, diluted with 50 mL water and extracted with dichloromethane (3 x 50 mL). The combined organic extracts are washed with water and 10% aqueous citric acid, dried over Na2S04 and concentration. Silica gel chromatography (5% to 25% ethyl acetate in hexanes) yielded [2-(2,4-Bis-trifluoromethyl- phenoxy) -ethyl]-carbamic acid tert-butyl ester 32 as a colorless, mobile oil: ‘H-NMR (400 MHz, CDC13) 8 = 7.61 (s, 1H), 7.00 (d, J = 8 Hz, 1H), 6.76 (d, J = 8 Hz, 1H), 5.10 (s, 1H), 4.26 (t, J = 4 Hz, 2H), 3.65 (m, 2H), 1.45 (s, 9H). 19F-NMR (376 MHz, CDC13) 8 =-61.5, – 62.0. No molecular ion could be obtained; a loss of tert-butyl group is observed: MS calculated for C11H10F6NO3 (M+H+-C4H8) 318.1, found 318.3.

The synthetic route of 327-75-3 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; IRM LLC; WO2005/113519; (2005); A1;,
Bromide – Wikipedia,
bromide – Wiktionary

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. 327-75-3, name is 1-Bromo-2,4-bis(trifluoromethyl)benzene, This compound has unique chemical properties. The synthetic route is as follows., COA of Formula: C8H3BrF6

[0199] To a solution of 95 (25.0 g, 0.10 mol) in anhy. THF (150 mL) was added NaOCH3 (7.0 g, 0.13 mol) at 0C. The mixture was then heated at 50C for 6 h. After cooling to 25C, the reaction mixture was quenched with sat. NH4C1, diluted with EtOAc, washed with brine, and concentrated in vacuo to afford crude methyl ether 96 (17.93 g, 73%) as a colorless liquid. This product was sufficiently pure to be used directly in subsequent reaction. 1H NMR (400 MHz, CDC13) : 8 7.83 (1H, s), 7.77 (1H, d, J = 8. 4 Hz), 7.09 (1H, d, J= 8.4 Hz), 3.97 (3H, s) ppm. A solution of methyl ether 96 (9.98 g, 0.04 mol) in anhyrous CH2C12 (150 mL) was cooled to-78C and treated with BBr3 (6.0 mL, 0.063 mol). The resultant brown mixture was stirred for 1 h at-78C, and then warmed up to 25C over 4 h, and then quenched with water. The organic layer was separated and washed with sat. NaHCO3 and brine, dried over Na2S04, concentrated to-13 mL in vacuo below 0C and used directly in the following substitution reaction. Take this solution (ca. 1.15 mL) and diluted with DMF (8 mL), and then treated with K2CO3 (1.27 g) and bromide 79 (1.72 g). The resultant mixture was stirred at room temperature for 1 h, diluted with EtOAc, washed with water and brine, dried over Na2S04, and concentrated in vacuum. The residue was purified by flash chromatography (5: 95 EtOAc/hexanes) on silica gel and then recrystallized with 10 % EtOAc/hexanes to give pure ester 97 as a white solid. 1H NMR (400 MHz, DMSO-d6) : No. 8. 60 (1H, d, J= 2.2 Hz), 8.17 (1H, dd, J= 8.6, 2.2 Hz), 7.96 (1H, s), 7.91 (1H, d, J= 8.6 Hz), 7. 84 (1H, d, J= 8.2 Hz), 7.74 (1H, t, J= 7.8 Hz), 7.38 (1H, d, J= 9.0 Hz), 6.40 (1H, s), 4.19 (2H, m), 1.11 (3H, t, J = 7.2 Hz) ppm.

According to the analysis of related databases, 327-75-3, the application of this compound in the production field has become more and more popular.

Reference:
Patent; METABOLEX, INC.; WO2005/80340; (2005); A1;,
Bromide – Wikipedia,
bromide – Wiktionary

327-75-3, A common heterocyclic compound, 327-75-3, name is 1-Bromo-2,4-bis(trifluoromethyl)benzene, molecular formula is C8H3BrF6, 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.

To a stirred solution of 3-methyl-4-nitro-lH-pyrazole (869 mg, 0.068 mmol, 1 equiv) l-bromo-2,4-bis(trifluoromethyl)benzene (2 g, 0.068 mmoles, leq) in DMF (20 mL) was added K CO (1.89 g, 0.0136 mmol, 2 equiv) and the reaction mixture was stirred for 15 minutes. Cul (0.026 g, 0.2eq, O.OOlmoles) and L-proline (0.317 g, 0.02 mmol, 0.4 equiv.) were added to the reaction mixture. The reaction mixture was allowed to stir for 24 hour at 100 C. Product formation was confirmed by LCMS. After completion of reaction, reaction mixture was diluted with water and extracted with ethyl acetate (3×100 mL). Combined organic extracts were washed with water (4×100 mL), dried over anhydrous NaSCL and concentrated under reduced pressure to obtain which was purified by flash chromatography (EtOAc/ Hexane) to obtain titile compound l-(2,4-bis(trifluoromethyl)phenyl)-3-methyl-4- nitro-lH-pyrazole (1.0 g). LCMS 339 [M+H] +.

The synthetic route of 1-Bromo-2,4-bis(trifluoromethyl)benzene has been constantly updated, and we look forward to future research findings.

Reference:
Patent; PRAXIS BIOTECH LLC; ALFARO, Jennifer; BELMAR, Sebastian; NUNEZ VASQUEZ, Gonzalo Esteban; PUJALA, Brahmam; SATHE, Balaji Dashrath; BERNALES, Sebastian; CHAKRAVARTY, Sarvajit; THAKRAL, Pooja; PATIDAR, Rajesh Kumar; (344 pag.)WO2019/195810; (2019); A2;,
Bromide – Wikipedia,
bromide – Wiktionary

327-75-3, The chemical industry reduces the impact on the environment during synthesis 327-75-3, name is 1-Bromo-2,4-bis(trifluoromethyl)benzene, I believe this compound will play a more active role in future production and life.

All experiments were performed in a previously-described quadrupole ion trap mass spectrometer (modified ThermoFinnigan LCQ DECA) equipped with electrospray ionization (ESI) [15, 17]. In a typical experiment, the dianion precursor was dissolved in methanol (10-4 M) and injected through the electrospray interface at flow rates ranging from 3 to 5 muL/min. The neutral reagents were mixed into the buffer gas by injecting a constant flow of reagent (20-400 muL/h) into a measured flow of helium (1000-1500 mL/min). Reactions were monitored as a function of time at various flow rates (pressures) of the reagent and branching ratios were determined. Time delays and reagent flows were adjusted to obtain plots that covered two to three half-lives of the reactant ion. Reported rate constants were measured at three different reagent flow rates and at least nine kinetic runs were collected on 2 or more days (>18 runs). In the past, we have shown that the ion trap gives reactivity at near ambient temperature [18]. All the arene reagents were obtained from commercial sources.

The chemical industry reduces the impact on the environment during synthesis 1-Bromo-2,4-bis(trifluoromethyl)benzene. I believe this compound will play a more active role in future production and life.

Reference:
Article; Eanes, Allison D.; Noin, Diogo O.; Kebede, Maheteme K.; Gronert, Scott; Journal of the American Society for Mass Spectrometry; vol. 25; 1; (2014); p. 10 – 17;,
Bromide – Wikipedia,
bromide – Wiktionary