Month: July 2021

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. 49764-63-8, name is 4,5-Dibromobenzene-1,2-diamine belongs to bromides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below. name: 4,5-Dibromobenzene-1,2-diamine

A mixture of 4,5-dibromo-o-phenylenediamine(40 mg, 0.15 mmol), 3-tert-butyl-5-nitrosalicylaldehyde(70 mg, 0.31 mmol) and Zn(OAc)2·2H2O (40 mg, 0.18 mmol) in MeOH (20 mL) was stirred for 4 h at room temperature. The orange product was then isolated by filtration and dried

The synthetic route of 49764-63-8 has been constantly updated, and we look forward to future research findings.

Reference:
Conference Paper; Anselmo, Daniele; Escudero-Adan, Eduardo C.; Martinez Belmonte, Marta; Kleij, Arjan W.; European Journal of Inorganic Chemistry; 29; (2012); p. 4694 – 4700;,
Bromide – Wikipedia,
bromide – Wiktionary

Electric Literature of 55289-36-6,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.

Tetrakis(triphenylphosphine)palladium(0) (Aldrich, catNo.216666: 300 mg, 0.3 mmol) was added to a mixture of 3-bromo-2-methylaniline (Aldrich, catNo.530018: 1000 mg, 5 mmol), phenylboronic acid (Aldrich, catNo.P20009: 600 mg, 5 mmol), 1,4-dioxane (20 mL, 200 mmol) and water (3 mL, 200 mmol), and the mixture was allowed to stir at 100 C. overnight. After concentration, the residue was dissolved in DCM and washed with brine. The organic layer was dried and concentrated to afford desired product as a brown solid, which was used in the next step without further purification. LC-MS calculated for C13H14N (M+H)+: m/z=184.1; found 184.1.

The synthetic route of 55289-36-6 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Incyte Corporation; Yu, Zhiyong; Wu, Liangxing; Yao, Wenqing; (44 pag.)US2018/16260; (2018); A1;,
Bromide – Wikipedia,
bromide – Wiktionary

Reference of 58971-11-2, 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 58971-11-2 as follows.

To a solution of 2-(3-bromophenyl)ethanamine (2 g, 10 mmol) in DCM (30 mL) were added Et3 (3 mL, 20.99 mmol) and AC2O (2 mL, 20.99 mmol). The reaction was stirred at rt overnight, then washed with H20 (50 mL x 3) followed by brine (50 mL x 3), dried over anhydrous a2S04, filtered and concentrated in vacuo to yield the crude product (2.42 g, 100%). MS (ESI, pos. ion) m/z: 242.0 [M + H]+; NMR (400 MHz, CDC13) delta (ppm): 7.36-7.33 (d, J= 9.2 Hz, 2H), 7.18-7.14 (t, J= 7.6 Hz, 1H), 7.12-7.10 (d, J= 8.0 Hz, 1H), 3.49-3.44 (t, J= 6.8 Hz, 2H), 2.79-2.76 (t, J= 7.2 Hz, 2H), 2.2 (s, 1H), 1.93 (s, 3H).

According to the analysis of related databases, 58971-11-2, the application of this compound in the production field has become more and more popular.

Reference:
Patent; CALITOR SCIENCES, LLC; SUNSHINE LAKE PHARMA CO., LTD; XI, Ning; WANG, Ruyong; WANG, Liang; WO2014/89324; (2014); A1;,
Bromide – Wikipedia,
bromide – Wiktionary

Adding a certain compound to certain chemical reactions, such as: 5153-40-2, name is 1-Bromo-2,3,4,5,6-pentamethylbenzene, 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 5153-40-2, Recommanded Product: 1-Bromo-2,3,4,5,6-pentamethylbenzene

Nl ,N5-bis(2.3.4.5.6-pentamethylphenyOpentane- 1 ,5-diamine (Example 8) [0082] In a drybox, 2,3,4,5,6-pentamethylbromobenzene (750.0 mg, 3.30 mmol), 1,5-pentanediamine (195.2 muL, 1.67 mmol), sodium tertbutoxide (396.6 mg, 4.13 mmol), 3.0 mL of dimethyoxyethane, and 10.0 mM Pd(OAc)2 / CyPF-Z-Bu (82.5 muL, 8.25 x 10-4 mmol) were added to a 20 mL scintillation vial equipped with a magnetic stirbar and sealed with a cap containing a PTFE septum. The reaction was placed into a temperature controlled aluminum heating block and stirred at 100 0C for 6 h. After cooling to room temperature, the reaction mixture was partitioned between 100 mL H2O/Diethyle ether (Et20) (1 : 1), the organic phase separated and dried over MgSO4, followed by the removal of all volatiles to afford 619 mg (95.0 %) of the title compound.|0083) 1H NuMR spectra were obtained at 400 MHz and recorded relative to residual protio solvent. 13C NuMR spectra were obtained at 101 MHz and recorded relative to the residual solvent resonance. The spectra recorded are as follows: 1H NMR (CDC13, 400 MHz, 22 0C): delta 1.50-1.71(m, 6H), 2.21 (s, 6H), 2.22 (s, 12H), 2.25 (s, 12H), 2.84 (t, J = 12 Hz, 4H), 2.88 (br s, 2H). 13C NMR (CDC13, 101 MHz, 22 0C): delta 14.8, 16.5, 16.9, 25.0, 30.9, 49.9, 126.8, 129.6, 132.9, 143.7.

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; UNIVATION TECHNOLOGIES, LLC; JOHNS, Adam, M.; WO2010/53696; (2010); A2;,
Bromide – Wikipedia,
bromide – Wiktionary

129316-09-2, name is 1,3-Dibromo-5-(tert-butyl)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. SDS of cas: 129316-09-2

17.7 g (60.47 mmol) of 1,3-dibromo-5-(tert-butyl)benzene was mixed with 200 ml of diethyl ether, and n-BuLi (1.6 M in hexane) was slowly added thereto at a temperature of -78C. After the reaction mixture was stirred at a temperature of -78C. for 1 hour, 15 g (72.6 mmol) of iodine mixed with 20 ml of THF was slowly added by drops thereto. The reaction mixture was stirred at room temperature for 16 hours. After the reaction was completed, the organic layer was extracted by using ethyl acetate and a sodium thiosulfate aqueous solution, dried by using magnesium sulfate, distilled under reduced pressure, and purified by liquid chromatography to obtain 18 g (54.5 mmol, yield: 60%) of Intermediate 5-6. LC-MS m/z=291 (M+H)+.

The synthetic route of 129316-09-2 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Samsung Electronics Co., Ltd.; Choi, Jongwon; CHO, Yongsuk; KOO, Hyun; PARK, Bumwoo; LEE, Sunghun; ISHIHARA, Shingo; KWAK, Yoonhyun; KWON, Ohyun; (138 pag.)US2019/194237; (2019); A1;,
Bromide – Wikipedia,
bromide – Wiktionary

Synthetic Route of 955959-84-9, 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. 955959-84-9, name is 4-(4-Bromophenyl)dibenzo[b,d]furan belongs to bromides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

In a stream of argon, 6.5 g of the intermediate-14′, 8.8 g of the intermediate-20′, 2.6 g of t-butoxy sodium, 92 mg of tris(dibenzylideneacetone)dipalladium, 42 mg of tri-t-butylphosphine, and 100 ml of dry toluene were loaded into a 300-ml three-necked flask, and then the mixture was subjected to a reaction at 80°C for 8 hours. After having been cooled, the reaction product was poured into 500 ml of water, and then the mixture was subjected to celite filtration. The filtrate was extracted with toluene, and was then dried with anhydrous magnesium sulfate. The dried product was concentrated under reduced pressure. The resultant coarse product was subjected to column purification, and was then recrystallized with toluene. The crystal was taken by filtration, and was then dried. As a result, 8.2 g of a pale yellow powder were obtained. The powder was identified as aromatic amine derivative (H-1′) by FD-MS analysis.

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-(4-Bromophenyl)dibenzo[b,d]furan, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; Idemitsu Kosan Co., Ltd.; EP2468725; (2012); A1;,
Bromide – Wikipedia,
bromide – Wiktionary

Synthetic Route of 126930-72-1, A common heterocyclic compound, 126930-72-1, name is 1-Bromo-4-dodecylbenzene, molecular formula is C18H29Br, 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.

Magnesium (3.3 g), tetrahydrofuran (20ml) were placed in aflask, and tetrahydrofuran (100ml) solution of 1-bromo-4-dodecylbenzene (40.1g) was added dropwise slowly at a rate to maintain reflux, and (4-dodecylphenyl) magnesium bromide was prepared. This was cooled in anice-water bath, and trimethyl borate (15.4g) was dropped slowly. After stirringfor 1 hour at room temperature, water and then concentrated hydrochloric acid(16 ml) were added, and stirred for 30 minutes. After extraction with ethylacetate, it was washed with water, dried over anhydrous sodium sulfate, andconcentrated to give (4-dodecylphenyl) boronic acid (32 g).

The synthetic route of 126930-72-1 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; JNC CORPORATION; KAWASHIMA, MASATOSHI; NOMURA, SHINTARO; (159 pag.)JP2015/203027; (2015); A;,
Bromide – Wikipedia,
bromide – Wiktionary

Adding a certain compound to certain chemical reactions, such as: 18087-73-5, name is 3-Bromoimidazo[1,2-b]pyridazine, 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 18087-73-5, HPLC of Formula: C6H4BrN3

To a 30 ml tube was added 3-ethynyl-4-methyl-N- [4- (4-methylpiperazin-1-ylmethyl) -3-trifluoromethylPhenyl] benzamide (126 mg, 0.3 mm & lt; 1 & gt;), 3 & lt; / RTI & gt; bromomethine [1,2_b] U daxazine (59 mg, 0.3 mmo 1), Pd (PPh3)(1 mg, 0.015 mmol), CuI (6 mg, 0.03 mmol), PCy3 (8 mg, 0.015 mmol), Cs2C0 (99 mg, 0.3 mmol)DMFlOml, replaced with argon for 5 minutes and then stirred at 80 C for 8 hours. With ethyl acetate (15 ml x 4), saturated with NaClSolution (30 ml). The organic layers were combined and dried over anhydrous Na2S04. The organic solution was concentrated under reduced pressure and the residue was passed throughThe title compound was obtained in a yield of 79%.

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; NANJING SANHOME PHARMACEUTICAL CO., LTD.; WANG, YONG; ZHAO, LIWEN; CHEN, HONGYAN; ZHANG, DI; XU, XIN; ZHANG, CANG; ZHANG, HONGXING; (9 pag.)CN103664951; (2016); B;,
Bromide – Wikipedia,
bromide – Wiktionary

10016-52-1, name is 2,8-Dibromodibenzo[b,d]furan, 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. Safety of 2,8-Dibromodibenzo[b,d]furan

2.75 g (10 mmol) of 4-phenylaminodibenzothiophene, 1.63 g (5.0 mmol) of 2,8-dibromodibenzofuran, 2.5 g (26 mmol) of sodium t-butoxide in a 50 ml four-necked flask,50 ml of dehydrated toluene was added and nitrogen bubbling was performed for 1 hour. Then, 3460 mg (0.5 mmol) of Pd2 (dba),290 mg (1.0 mmol) of tri-t-butylphosphonium tetrafluoroborate (t-Bu3PH + BF4-) was added, and the mixture was heated under reflux for 53 hours while stirring under a nitrogen stream. The formation of the desired product was confirmed by TLC and MS. The reaction solution was cooled to room temperature, and the organic layer was extracted with toluene, washed with brine, dried over anhydrous magnesium sulfate, filtered and concentrated to obtain a brown viscous product. The obtained viscous material was dissolved in 10 ml of toluene and packed in a column. The resultant was directly purified by silica gel column chromatography (developing solvent: toluene / hexane = 1/4) to obtain the desired product.Yield 1.92g, 54%

The synthetic route of 10016-52-1 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; National University Corporation Yamagata University; Sasabe, Hisahiro; Kido, Junji; Kamata, Takahiro; (21 pag.)JP2019/26556; (2019); A;,
Bromide – Wikipedia,
bromide – Wiktionary

Synthetic Route of 502496-36-8, 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 502496-36-8 as follows.

Reference Example 7: 6-Fluoroindazole-4-Boronate Ester (75) To a solution of 4-fluoro-2-nitrotoluene (3.44g) in trifluoroacetic acid (13mL) was added concentrated sulfuric acid (4mL) followed by N-bromosuccinimide (5.92g). The reaction mixture was stirred for 16 h and was then quenched with brine, extracted into ethyl acetate, and dried (MgSO4). The solvent was removed in vacuo to furnish crude l-bromo-5-fluoro-2-methyl-3-nitro-benzene (5.96g). To a solution of crude l-bromo-5-fluoro-2-methyl-3-nitro-benzene (5.96g) inMeOH (9OmL) was added concentrated hydrochloric acid (11.7mL) and iron (6.Ig) and the reaction mixture was heated to reflux. After 16 h, the mixture was cooled, diluted with DCM, washed with sodium carbonate solution, dried (MgSO4) and the solvent removed in vacuo. The residue was purified using flash chromatography to yield 3-bromo-5-fluoro-2-methyl-phenylamine (1.46g).To a solution of 3-bromo-5-fluoro-2-methyl-phenylamine (470mg) in dioxane (6mL) was added triethylamine (1.28mL), palladium acetate (25mg), 2- dicyclohexylphosphino biphenyl (161mg) and pinacol borane (1.001ml) and the mixture was heated to 8O0C for 4 h. The reaction mixture was cooled, diluted with chloroform, washed with brine, dried (MgSO4) and the solvent removed in vacuo. The residue was purified using flash chromatography to yield the desired title compound (466mg).

According to the analysis of related databases, 502496-36-8, the application of this compound in the production field has become more and more popular.

Reference:
Patent; PIRAMED LIMITED; WO2006/46031; (2006); A1;,
Bromide – Wikipedia,
bromide – Wiktionary