Category: 52548-00-2

In the next few decades, the world population will flourish. As the population grows rapidly and people all over the world use more and more resources, all industries must consider their environmental impact. 52548-00-2, name is 1-Bromo-4-fluoro-2,3-dimethylbenzene belongs to bromides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below. Formula: C8H8BrF

To a 250 ml-round bottle flask equipped with magnetic stir bar were added 1- Boc-piperizine (2.5 g, 13.42 mmol), 1-bromo-4-fluoro-2,3-dimethylbenzene (3.27 g, 16.11 mmol), Cs2CO3 (13.12 g, 40.3 mmol), and RuPhos Pd G2 (1.043 g, 1.342 mmol). To the mixture was charged dioxane (67.1 ml) at RT under N2. The mixture was stirred at RT while flushed with N2 for about 5 min and then warmed up to 90 C. The mixture was stirred at 90 C overnight. The mixture was cooled to RT, and partitioned between EtOAc and water (100 ml x 50 ml). The aqueous was extracted with EtOAc for three times (100 ml x 3). Organic phases were combined and washed with sat. NaCl, separated and dried over Na2SO4, filtered, concentrated, and followed by normal phase purfication (Isco system, 120 g Isco, RediSep gold column, 0-100% EtOAc / hexane as eluting solvent) to afford the title compound as a solid. LCMS m/z (M+H): 309.67

The synthetic route of 52548-00-2 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; MERCK SHARP & DOHME CORP.; CLAUSEN, Dane; CHEN, Ping; FRADERA, Xavier; GUO, Liangqin; HAN, Yongxin; HE, Shuwen; HUANG, Xianhai; KOZLOWSKI, Joseph; LI, Guoqing; MARTINOT, Theodore, A.; PASTERNAK, Alexander; VERRAS, Andreas; XIAO, Li; YU, Wensheng; ZHANG, Rui; (267 pag.)WO2020/112581; (2020); A1;,
Bromide – Wikipedia,
bromide – Wiktionary

Adding a certain compound to certain chemical reactions, such as: 52548-00-2, name is 1-Bromo-4-fluoro-2,3-dimethylbenzene, belongs to bromides-buliding-blocks 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 52548-00-2, Recommanded Product: 52548-00-2

B. 3-Fluoro-o-xylene-6-boronic acid To a 125 mL three-necked round-boftomed flask equipped with septum and N2 inlet were added 4.08 g (20 mmol) 3-fluoro-6-bromo-o-xylene and 20 mL dry tetrahydrofuran. The solution cooled to -70 C., and 9.6 mL (24 mmol) of a 2.5 M solution of butyl lithium in hexane was added slowly over 5 minutes. The reaction was stirred 5 minutes at -70 C., then 4.08 mL (24 mmol) triethyl borate added, and stirring continued at -70 C. for 5 minutes. The reaction was then allowed to warm to room temperature and stirred for 16 hours, then poured into dilute hydrochloric acid and extracted with ethyl acetate. The organic layer was washed with brine, dried over sodium sulfate, and evaporated. The residue was triturated with hexane to a white solid, 2.06 g (64%). 1H-NMR (delta, CDCl3): 2.22 (s, 3H), 2.30 (s, 3H), 6.7-7.3 (m, 2H). 13C-NMR (delta, CDCl3): 25.4, 26.3, 111.5, 111.7, 112.1, 112.3, 124.9, 126.0, 126.1, 130.8, 130.9,159.9,160.6, 162.3,163.0,.

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, 1-Bromo-4-fluoro-2,3-dimethylbenzene, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; VOLKMANN, ROBERT A.; LOWE III, JOHN A.; NOWAKOWSKI, JOLANTA; US2001/7873; (2001); A1;,
Bromide – Wikipedia,
bromide – Wiktionary

In the next few decades, the world population will flourish. As the population grows rapidly and people all over the world use more and more resources, all industries must consider their environmental impact. 52548-00-2, name is 1-Bromo-4-fluoro-2,3-dimethylbenzene belongs to bromides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below. COA of Formula: C8H8BrF

Step a. To a solution of 3-bromo-6-fluoro-o-xylene (CAS Number 52548-00-2; 3.00 g, 14.8 mmol) in CC1 (45 ml) was added NBS (5.780 g, 32.51 mmol) at rt. The reaction mixture was exposed to a UV light source which increased the temperature, in this manner the reaction mixture was heated at 85C for 2 h. The reaction mixture was cooled to rt and poured into saturated NaHC03 solution (100 ml). The resulting mixture was extracted with EtOAc (3 x 100 ml). The combined organic phase was washed with brine (100 ml), dried over Na2S04, filtered and concentrated under reduced pressure yielding 1-bromo-2,3-bis(bromomethyl)-4-fluorobenzene (5.80 g, 16.25 mmol). This material was directly used for next step without any further purification. LCMS: Method A, 2.489 min.

The synthetic route of 52548-00-2 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; MISSION THERAPEUTICS LIMITED; GIBSON, Karl Richard; JONES, Alison; KEMP, Mark Ian; MADIN, Andrew; STOCKLEY, Martin Lee; WHITLOCK, Gavin Alistair; WOODROW, Michael D; (241 pag.)WO2017/158388; (2017); A1;,
Bromide – Wikipedia,
bromide – Wiktionary

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 52548-00-2 as follows. Safety of 1-Bromo-4-fluoro-2,3-dimethylbenzene

6-Bromo-3-fluoro-o-xylene (5.00 g, 24.6 mmol) was dissolved in 75 mL carbon tetrachloride. N-Bromosuccinimide (8.76 g, 49.2 mmol) and benzoyl peroxide (0.089 g, 0.37 mmol) were added and the resulting white suspension was refluxed for 18 h. The reaction mixture was filtered and the filtrate concentrated to an oily suspension. The residue was purified by column chromatography on silica gel (eluting with hexanes) and concentrated to give 1-bromo-2,3-bis(bromomethyl)-4-fluorobenzene (8.40 g, 94% yield) as a colorless oil. 1H NMR (400 MHz, CDCl3, ppm) delta 7.55 (dd, J=8.9, 5.2 Hz, 1 H), 6.97 (t, J=8.9 Hz, 1 H), 4.78 (s, 3 H), and 4.67 (s, 3 H).

According to the analysis of related databases, 52548-00-2, the application of this compound in the production field has become more and more popular.

Reference:
Patent; Holloway, M. Katharine; Liverton, Nigel J.; Ludmerer, Steven W.; McCauley, John A.; Olsen, David B.; Rudd, Michael T.; Vacca, Joseph P.; McIntyre, Charles J.; US2007/27071; (2007); A1;,
Bromide – Wikipedia,
bromide – Wiktionary

Related Products of 52548-00-2, 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 52548-00-2 as follows.

PREPARATIVE EXAMPLE 44; .Ph In aBH4; Step i; A mixture of 3-bromo-6-fluoro-o-xyle?e (25.37g, 432 mmol) in anhydrous CCI4 (250 mL) was treated with NBS (44.5g, 864 mmol) and benzoyl peroxide (310 mg) and then heated at reflux overnight. The mixture was cooled to 0 C and filtered, washing with hexanes. The filtrate was concentrated and chromatographed (hexanes) to give 44A as an colorless oil (41.57g, with minor mono-bromo impurities).

According to the analysis of related databases, 52548-00-2, the application of this compound in the production field has become more and more popular.

Reference:
Patent; SCHERING CORPORATION; MCCORMICK, Kevin D.; DONG, Li; BOYCE, Christopher W; DE LERA RUIZ, Manuel; ZHENG, Junying; WON, Walter S.; WO2010/42475; (2010); A1;,
Bromide – Wikipedia,
bromide – Wiktionary