Month: July 2021

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

Step 1: Combine 2,4-difluorobromobenzene (6.00 g, 31 mmol) with AlCl3 (10.4 g, 34.3 mmol) and heat to 60° C. Add dropwise acetyl chloride (3.66 g, 47 mmol). Heat at 95° C. 1.5 h, cool to 0° C., and add ice-water, then conc. HCl (15 ml). Extract with ether, dry (MgSO4), concentrate and chromatograph on silica to obtain the ketone as a brown oil.

If you are interested in these compounds, you can also browse my other articles.Thank you for taking the time to read this article. I hope you enjoyed it.

Reference:
Patent; Neustadt, Bernard R.; Boyle, Craig D.; Chackalamannil, Samuel; Harris, Joel M.; Lankin, Claire M.; Liu, Hong; Shah, Unmesh; Stamford, Andrew; US2007/66620; (2007); A1;,
Bromide – Wikipedia,
bromide – Wiktionary

Some common heterocyclic compound, 460-00-4, name is 1-Bromo-4-fluorobenzene, molecular formula is C6H4BrF, 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-4-fluorobenzene

The reaction of 1-bromo-4-fluorobenzene(0.175 g, 1.0 mmol), aniline (0.093 g, 1.0 mmol), copper powder (0.0064 g, 0.1mmol), MI (0.036 g, 0.2 mmol), Cs2CO3 (0.720 g, 2.2 mmol), TBAHS (0.068 g, 0.2mmol) produced 0.148 g (79%) of 4-fluoro-N-phenylaniline as a brown oil.

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 460-00-4, its application will become more common.

Reference:
Article; Zhou, Qifan; Du, Fangyu; Chen, Yuanguang; Fu, Yang; Chen, Guoliang; Tetrahedron Letters; vol. 60; 29; (2019); p. 1938 – 1941;,
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. 73918-56-6, name is 2-(4-Bromophenyl)ethanamine belongs to bromides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below. SDS of cas: 73918-56-6

Preparation XXIV Ethyl [2-(4-bromophenyl)ethyl]carbamate . A solution of 4-bromophenethylamine (10.0 g, 50 mmol) and triethylamine (5.3 g, 52.5 mmol) in dichloromethane (200 ml) at 0C is treated with ethyl chloroformate (5.69 g, 52.5 mmol). The resulting solution is stirred at 0C for one hour and washed with saturated aqueous NaHCO3 solution (50 ml). The organic phase is dried (MgSO4) and concentrated. An oil is obtained (12.3 g, 90%).

The synthetic route of 73918-56-6 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; WARNER-LAMBERT COMPANY; EP421436; (1991); A2;,
Bromide – Wikipedia,
bromide – Wiktionary

Electric Literature of 57951-72-1, A common heterocyclic compound, 57951-72-1, name is 1-Bromo-2-cyclopropylethyne, molecular formula is C5H5Br, 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.

(0186) Lithium chloride (4.24 g) and 3 zinc powder (9.15 g) were dried under reduced pressure, and 4 tetrahydrofuran (THF) (100 mL), 5 1,2-dibromoethane (0.433 mL) and 6 trimethylchlorosilane (0.127 mL) were added thereto at room temperature. To the mixture was added dropwise a solution of 7 methyl (R)-3-iodo-2-methylpropionate (22.8 q) in THF (30 mL), and the mixture was stirred at 40 C. for 1.5 hr to prepare an organozinc reagent. In another reaction container were added 8 lithium chloride (7.63 g), 9 copper(I) cyanide (8.06 g) and THF (90 mL), and the mixture was stirred for 1 hr. The mixture was cooled to -10 C., and the aforementioned organo zinc reagent was added dropwise thereto. The reaction mixture was stirred at -10 C. for 10 min, cooled to -78 C., and a solution of 10 2-(bromoethynyl)cyclopropane (14.5 g) in THF (50 mL) was added dropwise. The mixture was stirred at the same temperature for 15 hr and poured into an aqueous ammonium chloride solution, and the mixture was extracted with ethyl acetate. The organic layer was washed with water, and the insoluble material was filtered off and washed with ethyl acetate. The filtrate was concentrated under reduced pressure, and the residue was purified by silica gel column chromatography (diethyl ether_hexane=1:30-1:5) to give the 11 title compound (9.93 g). Yield: 66%. (0187) 1H NMR (400 MHz, CDCl3) delta 3.69 (s, 3H), 2.59 (dq, J=6.8, 7.2 Hz, 1H), 2.46 (ddd, J=2.0, 6.0, 16.4 Hz, 1H), 2.29 (ddd, J=2.0, 7.8, 16.4 Hz, 1H), 1.23 (d, J=7.2 Hz, 3H), 1.22 (m, 1H), 0.71 (m, 2H), 0.60 (m, 2H). R

The synthetic route of 57951-72-1 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; AGC INC.; NIPPON ZOKI PHARMACEUTICAL CO., LTD.; YASUDA, Arata; MATSUMURA, Yasushi; SAWADA, Kazuyoshi; NANBA, Hiroyoshi; TAGUCHI, Kazuki; US2019/135743; (2019); 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. 393-36-2, name is 4-Bromo-3-(trifluoromethyl)aniline, A new synthetic method of this compound is introduced below., COA of Formula: C7H5BrF3N

3-Trifluoro4-bromo-aniline (5 g, 20.8 mmoL) in MeOH (10 mL) and THF (10 mL) was treated with NIS (5.16 g, 22.9 mmoL) at room temperature. After 2 hours, the reaction was quenched with saturated Na2S2O3. The solvent was removed and the residue was partitioned between CH2Cl2 and water. The organic layer was washed with brine and dried over anhydrous Na2SO4, then concentrated to yield a crude white solid. The crude material was purified using column chromatography (silica gel, 3:1 hexanes: EtOAc as eluent) to yield the title compound as a white solid. 1H NMR (CDCl3, 400 MHz) delta 7.88 (s, 1H), 6.98 (s, 1H), 4.45-4.18 (br, 5 s, 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; Lanter, James C.; Sui, Zhihua; Fiordeliso, James J.; Jiang, Weiqin; Zhang, Xuqing; US2005/250741; (2005); A1;,
Bromide – Wikipedia,
bromide – Wiktionary

Some common heterocyclic compound, 55289-36-6, name is 3-Bromo-2-methylaniline, molecular formula is C7H8BrN, 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 C7H8BrN

A mixture of 1-bromo-2-methyl-3-aminobenzene 25.0 g, triphosgene 60.0 g and toluene 400 mL was stirred withheating under ref lux for three hours. The reaction mixtures after standing to cool were concentrated under reduced pressure to give l-bromo-3-isocyanato-2- methylbenzene 30.3 g.?H NMR (CDC13) : 2.42(3H, 5), 7.00(1H, dt, J=0.5, 8.0Hz), 7.05(1H, dd, J=1.7, 8.0Hz), 7.39(1H,dd, 1.5, 7.7Hz).

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 55289-36-6, its application will become more common.

Reference:
Patent; SUMITOMO CHEMICAL COMPANY, LIMITED; YOSHIMOTO, Yuya; TAKAHASHI, Teruki; OOHIRA, Daisuke; AZUMA, Shuhei; WO2013/162077; (2013); 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, Product Details of 348-57-2

Combine 2,4-dibromofluorobenzene (6.00 g, 31 mmol) and AlCl3 (10.4 g, 34.3 mmol) and heat to 60° C. Add dropwise acetyl chloride (3.66 g, 47 mmol). Heat at 95° C. 1.5 h, cool to 0° C., and add ice-water, then conc. HCl (15 ml). Extract with ether, dry (MgSO4), concentrate and chromatograph on silica to obtain the ketone as a brown oil.

If you are interested in these compounds, you can also browse my other articles.Thank you for taking the time to read this article. I hope you enjoyed it.

Reference:
Patent; Schering Corporation; US2005/239795; (2005); A1;,
Bromide – Wikipedia,
bromide – Wiktionary

Reference of 7051-34-5, A common heterocyclic compound, 7051-34-5, name is (Bromomethyl)cyclopropane, molecular formula is C4H7Br, 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.

N-N(Bromomethyl)cyclopropane (0.95 mg, 6.70 mmol, 0.70 mL, 95 %) was added to a mixture of4-(4,4,5,5-tetramethyl-1 ,3,2-dioxaborolan-2-yl)-1 H-pyrazole (1 .00 g, 5.15 mmol) and caesium carbonate (3.49 mg, 10.72 mmol) in dry N,N-dimethylformamide (20 mL) at 0O. After stirring for 30 mm the ice-water bath was removed. The reaction mixture was stirred at room temperature overnight. The reaction mixture was diluted with ethyl acetate (150 mL) and washed with brine (3×100 mL). The organic layer was dried with sodium sulfate and concentrated in vacuo to afforded 1.30 g (4.38 mmol, 85% of theory) of the title compound. GO-MS (Method L9): R1 = 4.35 mm; mlz = 247 M1 H NMR (300 MHz, Ohloroform-d, Method M2) 6 7.81 (s, 1 H), 7.79 (s, 1 H), 3.99 (d, J = 7.1 Hz,2H), 1.32 (s, 12H), 1.27 (m, 1 H), 0.71 – 0.58 (m, 2H), 0.41 – 0.33 (m, 2H).

The synthetic route of 7051-34-5 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; BAYER ANIMAL HEALTH GMBH; KOeHLER, Adeline; WELZ, Claudia; BOeRNGEN, Kirsten; KULKE, Daniel; ILG, Thomas; KOeBBERLING, Johannes; HUeBSCH, Walter; SCHWARZ, Hans-Georg; GOeRGENS, Ulrich; EBBINGHAUS-KINTSCHER, Ulrich; HINK, Maike; NENNSTIEL, Dirk; RAMING, Klaus; ADAMCZEWSKI, Martin; BOeHM, Claudia; (269 pag.)WO2017/178416; (2017); A1;,
Bromide – Wikipedia,
bromide – Wiktionary

Reference of 126930-72-1,Some common heterocyclic compound, 126930-72-1, name is 1-Bromo-4-dodecylbenzene, molecular formula is C18H29Br, 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-bromo-4-dodecylbenzene (5.0 g, 15.4 mmol, 1.0 eq.), bispinacolato diboron (4.7 g, 1.2 eq.), potassium acetate (4.5 g, 3 eq.), and a bis(diphenylphosphino) ferrocene-palladium(II) dichloride dichloromethane complex (0.38 g, 0.03 eq.) were weighed and put into a 200 mL three-necked round bottom flask. Degassing under reduced pressure and nitrogen purge were sufficiently performed. Thereafter, 50 mL of cyclopentyl methyl ether was added thereto in a nitrogen atmosphere, and the mixture was refluxed and stirred. After completion of the reaction, heating was stopped, and the temperature of the reaction liquid was returned to room temperature. Extraction was performed with toluene, the organic solvent layers were then unified, anhydrous sodium sulfate was added thereto, and the mixture was allowed to stand for a while. Sodium sulfate was filtered off, and the solution was concentrated under reduced pressure. The mixture containing a desired product was further caused to pass through an activated carbon column chromatography, and a fraction containing a desired product was collected and concentrated under reduced pressure. Thus, a desired product ?PC12Bpin? was obtained.

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-dodecylbenzene, its application will become more common.

Reference:
Patent; Kwansei Gakuin Educational Foundation; JNC Corporation; HATAKEYAMA, Takuji; KONDO, Yasuhiro; NAKAMOTO, Keiichi; YANAI, Motoki; (190 pag.)US2018/94000; (2018); A1;,
Bromide – Wikipedia,
bromide – Wiktionary

Synthetic Route of 142808-15-9,Some common heterocyclic compound, 142808-15-9, name is 4-Bromo-2-fluorobenzotrifluoride, molecular formula is C7H3BrF4, 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 solution of cyclopropylmethanol (2.22 g, 31 mmol) in THF (100 mL) at 0C was added sodium hydride (60% dispersion in oil, 2.06 g, 51 mmol) in portions and stirred at room temperature for 30 minutes, followed by addition of 4-bromo-2-fluoro-l-(trifluoromethyl)benzeneare (295A) (5.0 g, 20.5 mmol). The mixture was stirred at room temperature for 16 hours, quenched with water (50 mL), and extracted with EtOAc (50 mL x 3). The combined organic phases was washed with brine (50 mL), dried over sodium sulphate, concentrated, and purified by column chromatography on silica gel (ethyl acetate in petroleum ether, 10% v/v) to furnish Compound 295B. LC-MS (ESI) m/z: non-ionizable compound under routine conditions used;1H-NMR (CDCb, 400 MHz): d (ppm) 0.39 (q, J= 4.9 Hz, 2H), 0.64 (q, J= 5.9 Hz, 2H), 0.81 – 0.91 (m, 1H), 3.91 (t, j= 8.1 Hz, 2H), 7.03 – 7.18 (m, 2H), 7.41 (d, 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 4-Bromo-2-fluorobenzotrifluoride, its application will become more common.

Reference:
Patent; BIOMARIN PHARMACEUTICAL INC.; WANG, Bing; CHAO, Qi; (737 pag.)WO2019/133770; (2019); A2;,
Bromide – Wikipedia,
bromide – Wiktionary