Month: May 2021

Reference of 952511-74-9, 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. 952511-74-9, name is 4-Bromo-3-methylbenzene-1,2-diamine belongs to bromides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

3: A mixture of 156 (28 g,140 mmol), formic acid (240 mL) and 37percent> concentrated HC1 (400 mL) was heated to 60 °C for 12 h, cooled in an ice-water bath, and the pH slowly adjusted to 8-9 with 28percent> concentrated NH4OH. The solid was collected by filtration, washed with water and dried in air to afford 25 g (98percent) of 5-bromo-4-methyl-lH-benzo[d]imidazole (158) as a yellow solid: MS (ESI) m/z = 213 [M+l]+.

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

Reference:
Patent; F. HOFFMANN-LA ROCHE AG; ALIAGAS-MARTIN, Ignacio; CRAWFORD, James; LEE, Wendy; MATHIEU, Simon; RUDOLPH, Joachim; WO2013/26914; (2013); 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. 5279-32-3, name is 5,6-Dibromobenzo[d][1,3]dioxole, A new synthetic method of this compound is introduced below., Application In Synthesis of 5,6-Dibromobenzo[d][1,3]dioxole

Step 1 5-(4-fluorophenyl)-6-[4-(methylthio)phenyl]-1,3-benzodioxole Under nitrogen, 1 g of Pd(PPh3)4 was added to a stirred solution of 4 g (14.3 mmol) of 5,6-dibromo-1,3-benzodioxole (Lancaster), 2.4 g (17.2 mmol) of 4-fluorophenyl boronic acid, and 2.87 g (17.2 mmol) of 4-methylthiophenylboronic acid (Example 1, Step 2) in 70 mL of toluene, 40 mL of ethanol, and 30 mL of 2M Na2 CO3. After vigorous stirring at reflux overnight, the solvent was removed in vacuo. The residue was dissolved in ethyl acetate, washed with water, and dried over Na2 SO4. Concentration in vacuo gave 6.9 g of 5-(4-fluorophenyl)-6-[4-(methylthio)phenyl]-1,3-benzodioxole as a semi-solid which was used without further purification.

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; G.D. Searle & Co.; US5739166; (1998); 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. 376646-62-7, name is (4-Bromo-2-methylphenyl)methanamine, A new synthetic method of this compound is introduced below., COA of Formula: C8H10BrN

To a round bottom flask were added di-tert-butyl dicarbonate (11.60 mL, 50.0 mmol), NaHCO3 (10.50 g, 125 mmol), (4-bromo-2-methylphenyl)methanamine (5 g, 24.99 mmol) and dioxane (54.9 mL). The reaction mixture was stirred at room temperature overnight, then filtered and concentrated. The residue was purified by (silica) column chromatography, eluting with a gradient of 5-30percent EtOAc in heptane to give the title compound as a white solid (6.581 g, 88percent). ESI-MS m/z [M+Hj 300.2.

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; JONES, Benjamin; KIRYANOV, Andre; KUEHLER, Jon; LANIER, Marion; MURPHY, Sean; ZHOU, Feng; (95 pag.)WO2019/60850; (2019); A1;,
Bromide – Wikipedia,
bromide – Wiktionary

Related Products of 875664-38-3,Some common heterocyclic compound, 875664-38-3, name is 1-Bromo-4,5-difluoro-2-methylbenzene, molecular formula is C7H5BrF2, 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.

1-47: A mixture of 2-bromo-4,5-difluorotoluene (4.00 g, 19.3 mmol), DIPEA (5.2 mL, 30.0 mmol), dichlorobis(benzonitrile)palladium(II) (269 mg, 0.700 mmol) and 1,1- bis(diphenylphosphino)ferrocene (dppf) (482 mg, 0.870 mmol) in absolute ethanol (50 mL) was placed in a sealed bomb with stirring and placed under 10 bars of carbon monoxide and heated to 135C for 4 h. The mixture was then cooled to RT, returned to atmospheric pressure and opened. The rxn mixture was concentrated and diluted with brine (100 mL) and extracted with EtOAc (3×50 mL). The combined organic layers were washed with brine (2×50 mL), dried over sodium sulfate, filtered and concentrated. The residue was purified by normal phase flash column chromatography on silica gel using 5-20% EtOAc in heptane to afford compound 1-47.

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-4,5-difluoro-2-methylbenzene, its application will become more common.

Reference:
Patent; EXELIXIS, INC.; XU, Wei; (170 pag.)WO2017/4609; (2017); A1;,
Bromide – Wikipedia,
bromide – Wiktionary

Reference of 30432-16-7, 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. 30432-16-7, name is 1,4-Dibromo-2,3-bis(bromomethyl)but-2-ene belongs to bromides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

Dissolve p-toluenesulfonamide (39.4g, 0.23mol) and potassium carbonate (202g, 1.45mol) in N,N-dimethylformamide (400mL), add 1,4-dibromo-2,3-bis(bromomethyl)but-2-ene (40g, 0.10mol), react at room temperature for 24 hours. Water (100 mL) was added to quench the reaction, stirred for 10 minutes, filtered, the filter cake was slurried with ethyl acetate (50 mL), filtered, and the filter cake was collected and dried to give the title compound 9b (39 g, yield 93%) as a white solid.

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, 1,4-Dibromo-2,3-bis(bromomethyl)but-2-ene, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; Guangdong Dongyangguang Pharmaceutical Co., Ltd.; Gu Zheng; Li Jianhao; Wang Weihua; Tan Haoxiong; Liu Jianyu; Zhang Yingjun; (73 pag.)CN111196806; (2020); 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. 51776-71-7, name is 1-Bromo-4-(difluoromethyl)benzene, A new synthetic method of this compound is introduced below., Computed Properties of C7H5BrF2

B. Synthesis of 2-[4-(difluoromethyl)phenyl]-4,4,5,5-tetramethyl-1,3,2-dioxaborolane[1,1′-Bis(diphenylphosphino)ferrocene]dichloropalladium(11) (25.25 g, 34.5 mmol) was added in one portion to a degassed mixture of 1-bromo-4-(difluoromethyl)benzene (160 g, 0.77 mol), 4,4,4′,4′,5,5,5′,5′-octamethyl-2,2′-bi-1,3,2-dioxaborolane (392.5 g, 1.55 mol) and potassium acetate (303 g, 3.09 mol) in 1,4-dioxane (2.42 L), and the reaction was heated to 100 C. for 18 hours. The mixture was then cooled to room temperature and filtered through Celite, washing with ethyl acetate (3 L). The filtrate was concentrated in vacuo to give a dark brown oil. The reaction was repeated an additional 3 times, on batches of 50 g, 160 g and 156 g of 1-bromo-4-(difluoromethyl)benzene (total starting material, 526 g, 2.54 mol), and the combined crude products were purified twice by chromatography on silica gel (Gradient: 0% to 3% ethyl acetate in heptane) to provide a yellow-white solid (803 g). This was recrystallized from methanol (1.6 L) at -20 C., and the filtrate was concentrated to one-half its original volume, cooled, and the resulting solid was collected by filtration. The combined solids (426 g) were recrystallized from heptane (500 mL) at -20 C., then melted and poured into methanol (200 mL) cooled in a methanol-ice bath. The mixture was broken up and filtered to yield C5 as a solid. Yield: 250.7 g, 0.987 mmol, 39%. 1H NMR (400 MHz, CDCl3) delta 1.37 (s, 12H), 6.65 (t, J=56.4 Hz, 1H), 7.52 (br d, J=8.1 Hz, 2H), 7.92 (br d, J=8.0 Hz, 2H).

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; Pfizer Inc.; US2012/214791; (2012); 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 41825-73-4 as follows. Recommanded Product: 2-Bromo-4,6-dimethylaniline

General procedure: To a stirred solution of the corresponding aniline (1 mmol),Cs2CO3 (2 mmol), and Pd(PPh3)4 (5 mol%) in toluene (20mL) at reflux and under nitrogen atmosphere, a solution ofN-Boc-pyrrol-2-yl boronic acid17 (1 mmol) in a mixture oftoluene (10 mL) and MeOH (3 mL) was added over 7 h. Themixture was stirred at reflux for 17 h, cooled, and the MeOHwas removed under reduced pressure. To the resultanttoluene suspension H2O (30 mL) was added, and the layerswere separated. The water layer was extracted with CH2Cl2(3 × 25 mL; or EtOAc for compound 5), the combinedorganic extracts were washed with H2O (30 mL), dried overMgSO4, filtered, and the solvent was evaporated underreduced pressure. The residue was purified by columnchromatography on silica gel using a suitable eluent asindicated below.

According to the analysis of related databases, 41825-73-4, the application of this compound in the production field has become more and more popular.

Reference:
Article; Petrov?i?, Matija; Ale?kovi?, Marija; Mlinari?-Majerski, Kata; Synlett; vol. 25; 19; (2014); p. 2769 – 2772;,
Bromide – Wikipedia,
bromide – Wiktionary

Electric Literature of 60956-23-2,Some common heterocyclic compound, 60956-23-2, name is 1,2-Dibromo-4-methylbenzene, molecular formula is C7H6Br2, 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: Fuel additive d was prepared according to the following scheme: The fuel additive was prepared using the following procedure: to a set of reaction tubes (dimensions 110 mm x 17 mm) was weighed the catalysts and bases by use of a Mettler Toledo FlexiWeigh automated solid dispenser. Separate tubes were used for the catalyst and for the base and internal standard. To the catalyst tube containing Pd2(dba)3 (14 mg, 0.016 mmol) and XPhos (30 mg, 0.062 mmol) was added tert- amyl alcohol (1 mL) and heated with stirring to 60 C for 0.5 hours before cooling to ambient temperature. To each reaction tube of pre-weighed potassium carbonate as base (94 mg, 0.68 mmol) and di-/er/-butyl biphenyl (12 mg) as internal standard was added tert- amyl alcohol (2 mL) with stirring and the liquid reagents dichlorotoluene (80 pL; 0.62 mmol) and ethanolamine (75 pL, 1.24 mmol) added. Subsequently, the 1 mL of pre-formed?Pd-XPhos? catalyst solution was charged to the main reaction tube and the resulting reaction mixture heated to 90 C with a chilled- condenser head block to avoid solvent loss. Sampling of the reaction was conducted manually extracting an aliquot by syringe or Eppendorf pipette at 0, 2 and 16 hours. The reaction was repeated using the same procedure, but modified in line with conditions in the following table:

The synthetic route of 60956-23-2 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; BP OIL INTERNATIONAL LIMITED; FILIP, Sorin, Vasile; GAUNT, Matthew; (23 pag.)WO2019/129594; (2019); A1;,
Bromide – Wikipedia,
bromide – Wiktionary

27976-27-8, name is (6-Bromohexyl)benzene, 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. Computed Properties of C12H17Br

(1) 2-(4-Benzyloxyphenyl)-5-methyl-1-{2-[4-(6-phenylhexyloxy)phenyl]ethyl}-1H-pyrrole A solution of 4-{2-[2-(4-benzyloxyphenyl)-5-methyl-1H-pyrrol-1-yl]ethyl}phenol (1.50 g, 3.91 mmol), 1-bromo-6-phenylhexane (1.42 g, 5.87 mmol) and potassium carbonate (811 mg, 5.87 mmol) in DMF (15 ml) was stirred at 80 C. for 12 hours. The reaction solution was poured into water and the mixture was extracted with ethyl acetate. The extract was washed with water and dried over magnesium sulfate anhydride, and solvent was removed under reduced pressure. The residue was purified by silica gel column chromatography (hexane:ethyl acetate=30:1) to give the object compound as an oily substance. 1.43 g (yield: 67.1%) 1H-NMR (CDCl3) delta; 1.22-1.79 (8H, m), 2.24 (3H, s), 2.57-2.72 (4H, m), 3.86-4.03 (4H, m), 5.11 (2H, s), 5.91 (1H, d, J=3.2 Hz), 6.03 (1H, d, J=3.2 Hz), 6.73 (2H, d, J=8.4 Hz), 6.82 (2H, d, J=8.4 Hz), 7.00 (2H, d, J=8.0 Hz),7.15-7.49 (12H, m). IR (KBr) cm-1; 1611, 1524, 1512, 1244, 1175, 752, 689.

The synthetic route of 27976-27-8 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Matsumoto, Takahiro; Katayama, Nozomi; Mabuchi, Hiroshi; US2003/144338; (2003); A1;,
Bromide – Wikipedia,
bromide – Wiktionary

Adding a certain compound to certain chemical reactions, such as: 202865-77-8, name is 2-Bromo-4-fluoro-6-methylaniline, 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 202865-77-8, Safety of 2-Bromo-4-fluoro-6-methylaniline

Referential Example 10 Synthesis of 2-Bromo-5-fluoro-4-methylaniline Iron powder (18.5 g) was added to a solution of 5-bromo-2-fluoro-4-nitrotoluene (9.7 g) in acetic acid (30 ml), and the mixture was stirred at 70 C. for 3 hours. The catalyst was removed by filtration through Celite, and the filtrate was washed with chloroform. The solvent and the like in the filtrate were distilled off under reduced pressure. The residue was subjected to column chromatography on silica gel to conduct elution with chloroform, thereby obtaining the title compound (7.9 g) as a red oil. 1 H-NMR (CDCl3) delta: 2.13(s,3H), 6.46(d,J=11 Hz,1H), 7.20(d,J=8 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, 2-Bromo-4-fluoro-6-methylaniline, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; Wakunaga Pharmaceutical Co., Ltd.; US6136823; (2000); A;,
Bromide – Wikipedia,
bromide – Wiktionary