Month: May 2021

Synthetic Route of 139155-55-8, 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. 139155-55-8, name is 1-Bromo-3-isobutylbenzene belongs to bromides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

Preparation 15 A mixture of 1-bromo-3-isobutylbenzene (3.16 g), magnesium (1.08 g), 1,2-dibromoethane (2.78 g) and iodine (10 mg) in tetrahydrofuran (10 ml) was refluxed for 1.5 hours. The mixture was cooled to 25 C., and a solution of 3-isobutylbenzaldehyde (2.40 g) in tetrahydrofuran (10 ml) was added at 25 C. After stirred for 1 hour at the same temperature, the mixture was poured into a mixture of ethyl acetate and 1N hydrochloric acid. The organic layer was separated, washed with water and brine, and dried over magnesium sulfate. After evaporation of the solvent, the residue was chromatographed on silica gel (200 g) eluding with 5% ethyl acetate in hexane to give bis(3-isobutylphenyl)methanol (2.90 g) as a colorless oil. NMR (CDCl3, delta): 0.89 (12H, d, J=7.5 Hz), 1.70-1.95 (2H, m), 2.46 (4H, d, J=7.5 Hz), 5.80 (1H, s), 6.97-7.09 (2H, m), 7.09-7.30 (6H, m)

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-3-isobutylbenzene, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; Fujisawa Pharmaceutical Co., Ltd.; US5212320; (1993); A;,
Bromide – Wikipedia,
bromide – Wiktionary

Related Products of 30432-16-7,Some common heterocyclic compound, 30432-16-7, name is 1,4-Dibromo-2,3-bis(bromomethyl)but-2-ene, molecular formula is C6H8Br4, 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.

In a two-necked flask, 4-hydroxybenzaldehyde (1) (0.02 mol) and KOH (0.02 mol) were dissolved in absolute ethyl alcohol (100 mL) and the solution was stirred for 30 minutes at room temperature. 1,4-dibromo-2,3-bis(bromomethyl)but-2-ene (2) (0.005 mol) was dissolved in absolute ethanol (25 mL) and added drop-wise to this solution at room temperature with the assistance of a dropping funnel. The mixture was then refluxed and stirred for 10 h. After completion of the reaction, the solution was filtered and the solid matter was obtained. It was washed with deionized water, ethanol and diethyl ether, subsequently. The solid matter was recrystallized using DMF/EtOH (1:1). The synthesized compound was dried with P2O5 in a vacuum oven. Some physical properties, the yield and FT-IR data for compound (3) are given in Table 1 and Table 2.

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 1,4-Dibromo-2,3-bis(bromomethyl)but-2-ene, its application will become more common.

Reference:
Article; Uysal, ?aban; Er, Mustafa; Tahtaci, Hakan; Synthetic Communications; vol. 46; 22; (2016); p. 1820 – 1832;,
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 6320-40-7 as follows. Application In Synthesis of 1,3,5-Tribromo-2-methylbenzene

Synthesis of Intermediates H and I; 2,4,6-tribromotoluene (3.3 g, 10 mmol) was dissolved in diethylether (30 ml). The reaction solution was cooled to -78 C., and n-butyllithium (4.4 ml, 11 mmol, 2.5M in hexane) was gradually added thereto. The reaction mixture was stirred at -78 C. for one hour, and copper chloride (II) (1.48 g, 11 mmol) was added thereto at -78 C. The reaction solution was stirred for five hours, and washed with distilled water and ethylacetate at room temperature. The obtained ethylacetate layer was dried over MgSO4 and then dried under a reduced pressure to obtain a crude product. The crude product was purified by silica gel column chromatography and recrystallized from dichloromethane and hexane to give intermediate H (622 mg, yield: 25%) and an intermediate I (746 mg, yield: 30%) as white solids. The structures of intermediates H and I were determined by 1H NMR. Intermediate H: 1H NMR (CDCl3, 300 MHz) delta (ppm) 7.74 (d, 4H), 7.18 (d, 4H), 2.06 (s, 6H); 13C NMR (CDCl3, 100 MHz) delta (ppm) 142.8, 134.9, 134.5, 131.1, 126.4, 119.4, 19.9. Intermediate I: 1H NMR (CDCl3, 300 MHz) delta (ppm) 7.60 (s, 4H), 2.61 (s, 6H); 13C NMR (CDCl3, 100 MHz) delta (ppm) 138.3, 137.2, 129, 9, 125.8, 23.5.

According to the analysis of related databases, 6320-40-7, the application of this compound in the production field has become more and more popular.

Reference:
Patent; Samsung SDI Co., Ltd.; US2008/174237; (2008); A1;,
Bromide – Wikipedia,
bromide – Wiktionary

These common heterocyclic compound, 21865-50-9, name is 6-Bromo-2,3,4,9-tetrahydro-1H-carbazole, 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. Computed Properties of C12H12BrN

In a 1 L round-bottom flask, 60.0 g (0.240 mol) of synthesized in [Scheme 2], 73.4 g (0.360 mol) of iobenzene, 2.3 g (0.012 mol) of copper iodide (CuI),Tripotassium phosphate (K3PO4) 106.96 g (0.504 mol),54.8 g (0.480 mol) of trans-1,2-cyclohexanediamineAnd 300.0 ml of 1,4-dioxane was added and refluxed for 12 hours. After the reaction was completed, the mixture was cooled to room temperature, extracted with 1 L of water, and the organic layer was anhydrous and concentrated under reduced pressure. Then, 72.0 g (yield 92.0%) of was obtained by using an adsorption column chromatography.

The synthetic route of 6-Bromo-2,3,4,9-tetrahydro-1H-carbazole has been constantly updated, and we look forward to future research findings.

Reference:
Patent; SFC Ltd.; Kim Si-in; Kim Nam-i; (52 pag.)KR102017507; (2019); B1;,
Bromide – Wikipedia,
bromide – Wiktionary

Electric Literature of 106-37-6, As we all know, there are many different methods for the synthesis of a compound, and people can choose the synthesis method that suits their own laboratory according to the actual situation. 106-37-6 name is 1,4-Dibromobenzene, This compound is widely used in many fields, so it is necessary to find a new synthetic route. The downstream synthesis method of this compound is introduced below.

Under nitrogen environment, compound G was dissolved in tetrahydrofuran / toluene (5: 1) and then 0.9 equivalent of compound F was added. After 4.4 equivalent of Potassium carbonate was dissolved in DI water, 0.05 equivalent of Pd (0) was added. The reaction mixture was then refluxed at 80 C. for 24 hours and the reaction was terminated. After extraction with organic solvent, the organic solvent was removed. Compound H was obtained by reprecipitation after a column.

At the same time, in my other blogs, there are other synthetic methods of this type of compound, 1,4-Dibromobenzene, and friends who are interested can also refer to it.

Reference:
Patent; LG Display Co., Ltd.; Yoon Gyeong-jin; Noh Hyo-jin; (33 pag.)KR2019/63923; (2019); A;,
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. 86845-28-5, name is 1-Bromo-3-methyl-5-(trifluoromethyl)benzene, A new synthetic method of this compound is introduced below., HPLC of Formula: C8H6BrF3

1-ethenyl-3-methyl-5-(trifluoromethyl)benzene To 1-bromo-3-methyl-5-(trifluoromethyl)benzene (500 mg, 2.51 mmol) was added THF (5 mL), aqueous tribasic potassium phosphate (2.0 M, 4.18 mL, 8.37 mmol), 2-ethenyl-4,4,5,5-tetramethyl-1,3,2-dioxaborolane (387 mg, 2.51 mmol), palladium(II) acetate (47 mg, 0.209 mmol), and 1,1′-bis(di-t-butylphosphino)ferrocene (99 mg, 0.209 mmol). The system was flushed with nitrogen gas and was heated at 80 C. for 1 hour. The reaction was filtered and then diluted with ethyl acetate and water. The organic layer was dried over sodium sulfate, filtered and concentrated. The crude product was purified by preparative TLC to yield 1-ethenyl-3-methyl-5-(trifluoromethyl)benzene (300 mg, 1.61 mmol). 1H NMR (500 MHz, CDCl3) delta7.47 (s, 1H), 7.40 (s, 1H), 7.34 (s, 1H), 6.76 (m, 1H), 5.85 (d, J=17.6 Hz, 1H), 2.43 (s, 1H).

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; Shao, Pengcheng Patrick; Sun, Wanying; Katipally, Revathi Reddy; Vachal, Petr; Ye, Feng; Liu, Jian; Sha, Deyou; US2013/109649; (2013); 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 89523-51-3 as follows. Product Details of 89523-51-3

(A-4) Synthesis of benzo(c)phenanthrene-5-boronic acid Under the atmosphere of argon, 10.1g of 5-bromobenzo[c]phenanthrene was placed in a flask, and 400 mL of dehydrated ether was added. The reaction solution was cooled to -40C, and 22 mL of a hexane solution of 1.6 M n-butyl lithium was added. The resultant was heated to 0C, and stirred for 1 hour. The reaction solution was cooled to -60C, and 10 mL of a dehydrated ether solution of 14.4g of triisopropyl borate was added dropwise. While heating the reaction solution to room temperature, stirring was continued for 5 hours. 10 mL of a 10% aqueous hydrochloric acid solution was added, followed by stirring for 1 hour. An aqueous phase was removed, and an organic phase was washed with water and saturated saline, and dried with magnesium sulfate. After filtering off magnesium sulfate, the organic phase was concentrated. The resulting solids were washed with hexane, whereby 5.37g (yield 60%) of benzo[c]phenanthrene-5-boronic acid as an intended product was obtained.

According to the analysis of related databases, 89523-51-3, the application of this compound in the production field has become more and more popular.

Reference:
Patent; Idemitsu Kosan Co., Ltd.; EP2524913; (2012); A1;,
Bromide – Wikipedia,
bromide – Wiktionary

Reference of 105309-59-9, A common heterocyclic compound, 105309-59-9, name is Tetrakis(4-bromophenyl)methane, molecular formula is C25H16Br4, 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.

General procedure: A solution of Ar-X (2.0 mmol), TeocNHOTBS (3; 640 mg, 2.2 mmol), Bippyphos (2; 51 mg, 0.10 mmol), and Pd2dba3 (23 mg, 0.025 mmol) in toluene (8 mL) was treated with Cs2CO3 (1.3 g, 4.0 mmol). N2 was bubbled through the mixture for 30 min, and then the mixture was heated and stirred at 80 C for 16 h under N2. The resulting mixture was purified directly by column chromatography (EtOAc/hexanes).

The synthetic route of 105309-59-9 has been constantly updated, and we look forward to future research findings.

Reference:
Article; Beaudoin, Daniel; Wuest, James D.; Tetrahedron Letters; vol. 52; 17; (2011); p. 2221 – 2223;,
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. 51776-71-7, name is 1-Bromo-4-(difluoromethyl)benzene belongs to bromides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below. category: bromides-buliding-blocks

Example 38; 4-(4-Difluoromethyl-phenoxy)-2,2-dimethyl-2,3-dihydro-benzofuran-6-carboxylic acid (1-methyl-1H-pyrazol-3-yl)-amide; A mixture of 4-hydroxy-2,2-dimethyl-2,3-dihydro-benzofuran-6-carboxylic acid (1-methyl-1H-pyrazol-3-yl)-amide (31a) (102 mg, 0.36 mmol), 1-bromo-4-difluoromethyl benzene (110 mg, 0.53 mmol), Cs2CO3 (174 mg, 0.53 mmol) and CuI (1 mg) in DMF (5 mL) was heated for 2 hr at 160 C. in the microwave. The mixture was filtered and the filtrate was purified by reverse phase chromatograph to give a white solid (18 mg, 12% yield). 1H NMR (400 MHz, CDCl3) delta 9.92 (d, J=2.02 Hz, 1H) 8.52 (s, 1H) 7.72 (dd, J=10.36, 1.77 Hz, 1H) 7.64 (d, J=8.34 Hz, 1H) 7.28 (s, 1H) 7.09 (t, J=7.96 Hz, 1H) 7.05 (s, 1H) 6.97 (s, 1H) 6.77 (d, J=2.02 Hz, 1H) 3.78 (s, 3H) 2.98 (s, 2H) 1.51 (s, 6H); LCMS for C22H21F2N3O3 m/z 414.00 (M+H)+.

The synthetic route of 51776-71-7 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Pfizer Inc.; US2008/280875; (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. 875664-41-8, name is 3-Bromo-4,5-difluoroaniline, A new synthetic method of this compound is introduced below., Computed Properties of C6H4BrF2N

To a solution of 4-amino-A/-hydroxy-1 ,2,5-oxadiazole-3-carbimidoyl chloride (Int 7a) (250 mg, 1 .54 mmol) and 3-bromo-4,5-difluoroaniline (320 mg, 1 .54 mmol) in H20 and THF (12 mL, 1 :1 ) was added NaHC03 (194 mg, 2.31 mmol). The mixture was stirred at 65 C for 2 hours. Then the mixture was diluted with EtOAc (50 mL). The organic layer was washed with water (30 mL) and brine (30 mL), dried over Na2S04 and concentrated. The residue was purified by column chromatography on silica gel (PE: EtOAc = 5:1 ) to give the title compound as a white solid.

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; PHENEX DISCOVERY VERWALTUNGS-GMBH; STEENECK, Christoph; KINZEL, Olaf; ANDERHUB, Simon; HORNBERGER, Martin; KLEYMANN, Gerald; HOFFMANN, Thomas; (191 pag.)WO2018/83241; (2018); A1;,
Bromide – Wikipedia,
bromide – Wiktionary