Category: 348-57-2

These common heterocyclic compound, 348-57-2, name is 1-Bromo-2,4-difluorobenzene, 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: 1-Bromo-2,4-difluorobenzene

2,4-difluorobromobenzene (3 g, 15.5 mmol) and 260 mg of iron filings were placed in a two-neck flask, and 15 ml of dichloromethane was then added thereto. The two-neck flask was cooled in an ice bath, and a solution including bromine (1 ml, 18.7 mmol) and 15 ml of dichloromethane was added dropwise to the two-neck flask using an isobaric funnel. Next, the contents in the two-neck flask were heated under reflux for 3 hours. During heating, brown gas was produced. Then, the temperature was reduced to 20 C., and 50 ml of a sodium metabisulfite (Na2S2O5) aqueous solution (10%) was mixed with the contents in the two-neck flask by stirring for 1 hour for terminating the reaction therein. Thereafter, the contents in the two-neck flask were washed several times with deionized water to collect an organic layer, the organic layer was dehydrated using sodium sulfate (Na2SO4), and the solvent in the organic layer was removed, followed by column chromatography (SiO2, n-hexane), thereby obtaining white crystals (3.5 g, 83% yield). (0067) The spectrum analysis for the white crystals is: 1H NMR (400 MHz, CDCl3): delta 7.74 (t, J=7.6 Hz, 1H), 6.96 (t, J=8.0 Hz, 1H); 19F NMR (376 MHz, CDCl3, 298 K): delta -103.8 (dd, J=7.5 Hz, J=7.5 Hz). The white crystals were confirmed to be Compound L3-1 having a chemical structure represented by

The synthetic route of 1-Bromo-2,4-difluorobenzene has been constantly updated, and we look forward to future research findings.

Reference:
Patent; NATIONAL TSING HUA UNIVERSITY; Chi, Yun; Tong, Bi-Hai; Duan, Tai-Nan; Ku, Hsiao-Yun; Chen, I-Jen; US9219237; (2015); B1;,
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. 348-57-2, name is 1-Bromo-2,4-difluorobenzene, This compound has unique chemical properties. The synthetic route is as follows., Formula: C6H3BrF2

To a suspension of l-bromo-2,4-difluorobenzene (lOg, 52.1mmol, l.Oeq) in cold H2SO4 (37.9mL) was added Conc.HN03 (33.3mL) in a dropwise manner keeping the internal temp 20°C, stirred for 10 min at 0°C then, the reaction mixture was poured into a mixture of diethyl ether (250mL) and ice water (250mL) with vigorous stirring. The organic layer was separated and the aqueous layer was again extracted with Et20 (250mL). The combined organic layer was washed with Satd. sodium bicarbonate (2 X 200 mL) followed by satd. brine (2 X 200 mL) solution. The separated organic layer was dried over Na2S04 and concentrated under reduced pressure to give crude product which was purified by column chromatography (SiO 100-200 mesh) using 15percent EtOAc in pet ether as an eluent to give l-bromo-2,4-difluoro-5 -nitrobenzene (52g, 72percent yield) as a yellow color liquid. LCMS: M+H]+ 272.23.

According to the analysis of related databases, 348-57-2, the application of this compound in the production field has become more and more popular.

Reference:
Patent; ONTARIO INSTITUTE FOR CANCER RESEARCH (OICR); AL-AWAR, Rima; ZEPEDA-VELAZQUEZ, Carlos Armando; PODA, Gennady; ISAAC, Methvin; UEHLING, David; WILSON, Brian; JOSEPH, Babu; LIU, Yong; SUBRAMANIAN, Pandiaraju; MAMAI, Ahmed; PRAKESCH, Michael; STILLE, Julia Kathleen; (1053 pag.)WO2017/147700; (2017); A1;,
Bromide – Wikipedia,
bromide – Wiktionary

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. 348-57-2, name is 1-Bromo-2,4-difluorobenzene, A new synthetic method of this compound is introduced below., Application In Synthesis of 1-Bromo-2,4-difluorobenzene

39 mmol (7.52 g) of 1-bromo-2,4-difluorobenzene were loaded into a 100-ml flask, and the temperature of the 1-bromo-2,4-difluorobenzene was heated to 60C. Next, 0.15 g of iron was added, and then 39 mmol (6.23 g) of bromine were dropped over 3 hours while the temperature of the mixture was kept at 60C. After the completion of the dropping, the resultant was further subjected to a reaction at 60C for 2 hours. After the temperature of the resultant reaction liquid had been cooled to room temperature, the reaction liquid was charged into a cold aqueous solution of sodium hydroxide, and the reaction product was extracted with hexane. An organic layer was washed with pure water and a saturated sodium chloride solution, and was dehydrated with anhydrous sodium sulfate. After that, the solvent was removed. The resultant residue was purified by means of silica gel chromatography (developing solvent: hexane), whereby 8.81 g of a compound A as colorless oil were obtained (84% yield).

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; Chuo University; Idemitsu Kosan Co., Ltd.; EP1961743; (2008); A1;,
Bromide – Wikipedia,
bromide – Wiktionary

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. 348-57-2, name is 1-Bromo-2,4-difluorobenzene, A new synthetic method of this compound is introduced below., COA of Formula: C6H3BrF2

Example 67; 6-fluoro-9-furan-3-yl-2,3,4,5-tetrahydro-1,4-benzoxazepine hydrochloride; (1) 3-bromo-2,6-difluorobenzoic acid; To a mixed solution of 1.6N solution of n-butyllithium in hexane (9.4 ml, 15.0 mmol) and tetrahydrofuran (20 ml) were successively added 2,2,6,6-tetramethylpiperidine (2.50 ml, 15.0 mmol) and 1-bromo-2,4-difluorobenzene (2.90 g, 15.0 mmol) at -78°C, and the mixture was stirred at -78°C for 1 hr. The pulverized dry ice (5 g) was added, and the mixture was stirred at -78°C for 2 hr. Saturated aqueous ammonium chloride solution (5 ml) was added to the reaction mixture, and the mixture was stirred at room temperature for 30 min. Water (10 ml) and 1N hydrochloric acid (30 ml) were added, and the mixture was extracted with ethyl acetate. The extract was washed with water and dried over anhydrous magnesium sulfate. The solvent was evaporated under reduced pressure. Hexane was added to the residue, and desired product (2.30 g, 64.6percent) was collected by filtration as a solid. 1H-NMR (CDCl3) delta; 6.91-6.97 (1H, m), 7.66-7.73 (1H, m).

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; Takeda Pharmaceutical Company Limited; EP2123644; (2009); 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. 348-57-2, name is 1-Bromo-2,4-difluorobenzene, This compound has unique chemical properties. The synthetic route is as follows., name: 1-Bromo-2,4-difluorobenzene

Iron powder (16.49 g, 291 mmol) is added to 1-bromo-2,4-difluorobenzene (110 mL, 968 mmol) in 1,2-dichloroethane (968 mL) in a 3-neck flask at ambient temperature under a stream of nitrogen. A solution of bromine (59.7 mL, 1.16 mol) in 1,2-dichloroethane (968 mL) is added dropwise over 1 hour and the reaction mixture is stirred at ambient temperature for 18 h. The reaction mixture is cooled to 0 C. and a saturated aqueous solution of sodium bisulfate (1.11 L, 533 mmol) is added portionwise and the mixture is separated. The aqueous phase is extracted with dichloromethane. The organic layer is washed with a saturated aqueous solution of sodium bicarbonate, water, and brine. The organic layer is dried over sodium sulfate, and the solvent is removed under reduced pressure to give a residue purified with a pad of silica using diethyl ether to give the title compound (229 g, 76%). 1H NMR (400 MHz, CDCl3) delta 7.70 (dd, J=4.6, 6.8 Hz, 1H), 6.95-6.92 (m, 1H).

According to the analysis of related databases, 348-57-2, the application of this compound in the production field has become more and more popular.

Reference:
Patent; ELI LILLY AND COMPANY; US2011/9395; (2011); A1;,
Bromide – Wikipedia,
bromide – Wiktionary

Adding a certain compound to certain chemical reactions, such as: 348-57-2, name is 1-Bromo-2,4-difluorobenzene, 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 348-57-2, HPLC of Formula: C6H3BrF2

To a 0 C. mixture of 1-bromo-2,4-difluorobenzene (20.0 g; 11.7 mL; 0.100 mol) and H2SO4 (76.8 mL) was added HNO3 (68.0 mL) over 45 min at such a rate that the internal temperature was < 7 C. The resulting mixture was stirred for 1 h at 0 C., poured into ice water (400 mL), stirred vigorously for 2-3 min and extracted with CH2Cl2 (400 mL). The CH2Cl2 extract was washed with brine (1?500 mL), dried over Na2SO4, filtered and evaporated to give the product as a yellow oil (23.5 g, 95percent). 1H NMR (300 MHz, CDCl3) ? 7.14 (ddd, J=0.3, 7.8, 9.9 Hz, 1H), 8.39 (t, J=7.2 Hz, 1H). At the same time, in my other blogs, there are other synthetic methods of this type of compound, 1-Bromo-2,4-difluorobenzene, and friends who are interested can also refer to it. Reference:
Patent; Synaptic Pharmaceutical Corporation; US2005/154020; (2005); A1;,
Bromide – Wikipedia,
bromide – Wiktionary

348-57-2, name is 1-Bromo-2,4-difluorobenzene, belongs to bromides-buliding-blocks compound, is considered to be a conventional heterocyclic compound, which is widely used in drug synthesis. The chemical synthesis route is as follows. COA of Formula: C6H3BrF2

EXAMPLE 16 Preparation of 4-(2,4-difluorophenyl)-anisole from 4-methoxyphenylmagnesiumbromide and palladium acetate/triphenylphosphine (0.1percent) A suspension of magnesium turnings (13.5 g; 555 mmoles–Janssen) in tetrahydrofuran (132.9 g) was heated at 65¡ã C. under stirring and under nitrogen. Then, iodine (0.35 g) and, after 30 minutes, 4-bromoanisole (102.65 g; 549 mmoles), in 1 hour, were added to the reaction mixture. At the end of the addition, the reaction mixture was kept at 75¡ã C. for 1 hour and, then, decanted obtaining a solution of 4-methoxyphenylmagnesiumbromide (solution A). A mixture of 1-bromo-2,4-difluorobenzene (100 g; 518 mmoles), palladium acetate (0.11644 g; 0.519 mmoles–Janssen) and triphenylphosphine (0.54356 g; 2.07 mmoles–Fluka) was de-aerated by vacuum/nitrogen at 25¡ã C. The mixture was heated at 85¡ã C., kept under stirring for 15 minutes and, then, solution A was added in 6 hours. At the end of the addition, the reaction mixture was kept at 85¡ã C. for 30 minutes. After cooling at 60¡ã C., a solution of 37percent hydrochloric acid (17.5 ml) in water (88 ml) was added in 20 minutes. The mixture was cooled at 40¡ã C. and the phases were separated. The solvent of the organic phase was evaporated under reduced pressure obtaining the desired compound (113 g; HPLC titre 93.71percent; 93percent yield).

The synthetic route of 348-57-2 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Zambon Group S.p.A.; US5312975; (1994); A;,
Bromide – Wikipedia,
bromide – Wiktionary

These common heterocyclic compound, 348-57-2, name is 1-Bromo-2,4-difluorobenzene, 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. Quality Control of 1-Bromo-2,4-difluorobenzene

1-Bromo-2,4-difluoro-5-nitrobenzene: To a 0¡ã C. mixture of 1-bromo-2,4-difluorobenzene (20.0 g; 11.7 mL; 0.100 mol) and H2SO4 (76.8 mL) was added HNO3 (68.0 mL) over 45 min at such a rate that the internal temperature was <7¡ã C. The resulting mixture was stirred for 1 h at 0¡ã C., poured into ice water (400 mL), stirred vigorously for 2-3 min and extracted with CH2Cl2 (400 mL). The organic layers were washed with brine (1.x.500 mL), dried over Na2SO4, filtered and evaporated to give the product as a yellow oil (23.5 g, 95percent). 1H NMR (CDCl3) delta 8.39 (t, J=7.2 Hz, 1H), 7.14 (ddd, J=0.3, 7.8, 9.9 Hz, 1H). The synthetic route of 1-Bromo-2,4-difluorobenzene has been constantly updated, and we look forward to future research findings. Reference:
Patent; Marzabadi, Mohammad R.; Chen, Chien-An; Jiang, Yu; Lu, Kai; Andersen, Kim; US2006/79522; (2006); A1;,
Bromide – Wikipedia,
bromide – Wiktionary

Adding a certain compound to certain chemical reactions, such as: 348-57-2, name is 1-Bromo-2,4-difluorobenzene, 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 348-57-2, Recommanded Product: 1-Bromo-2,4-difluorobenzene

Preparation 131 ,5-dibromo-2,4-difluorobenzeneTo a solution of l-bromo-2,4-difluorobenzene (19.3 mL, 171 mmol) in CH2CI2 (100 mL) was added iron (3.15 g,56 mmol). To this stirred suspension was added a solution of bromine (1 1 mL, 214 mmol) in CH2CI2 (25 mL) drop wise over 30 min. The resulting mixture was stirred at rt overnight. The reaction mixture was slowly poured into saturated aqueous Na2S203 (200 mL), and the resulting mixture was stirred at rt for 30 min. This was extracted with CH2C12 (3 x 80 mL). The combined extracts were washed with brine, dried over MgS04, filtered and concentrated in vacuo to give 1,5-dibromo- 2,4-difluorobenzene (40 g, 86 % yield) as a brown oil. XH NMR (500 MHz,CHLOROFORM-d) delta 7.79 (t, J=7.0 Hz, 1H), 7.00 (t, J=8.2 Hz, 1H).

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-2,4-difluorobenzene, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; BRISTOL-MYERS SQUIBB COMPANY; WU, Yong-Jin; WO2012/162334; (2012); A1;,
Bromide – Wikipedia,
bromide – Wiktionary

Synthetic Route of 348-57-2,Some common heterocyclic compound, 348-57-2, name is 1-Bromo-2,4-difluorobenzene, molecular formula is C6H3BrF2, 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.

Preparation 1 1 ,5-dibromo-2,4-difluorobenzene To a solution of l-bromo-2,4-difluorobenzene (19.3 mL, 171 mmol) in CH2CI2 (100 mL) was added iron (3.15 g,56 mmol). To this stirred suspension was added a solution of bromine (1 1 mL, 214 mmol) in CH2CI2 (25 mL) drop wise over 30 min. The resulting mixture was stirred at rt overnight. The reaction mixture was slowly poured into saturated aqueous Na2S203 (200 mL), and the resulting mixture was stirred at rt for 30 min. This was extracted with CH2C12 (3 x 80 mL). The combined extracts were washed with brine, dried over MgS04, filtered and concentrated in vacuo to give 1,5-dibromo- 2,4-difluorobenzene (40 g, 86 % yield) as a brown oil. XH NMR (500 MHz, CHLOROFORM-d) delta 7.79 (t, J=7.0 Hz, 1H), 7.00 (t, J=8.2 Hz, 1H).

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 1-Bromo-2,4-difluorobenzene, its application will become more common.

Reference:
Patent; BRISTOL-MYERS SQUIBB COMPANY; WU, Yong-Jin; GUERNON, Jason M.; WO2014/98831; (2014); A1;,
Bromide – Wikipedia,
bromide – Wiktionary