Bromides-buliding-blocks

7745-91-7, Adding a certain compound to certain chemical reactions, such as: 7745-91-7, name is 3-Bromo-4-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 7745-91-7.

Step 1 : 3-bromo-4-methylaniline (1.0 equiv), hexane-2,5-dione (1.1 equiv.) and -TsOH (0.05 equiv.) were combined in toluene (0.4 M) and the mixtore heated in Dean- Stark at 150 C. After 35 min, the reaction mixture was cooled to room temperature. The reaction mixture was let to age at room temperature for 60 h and then concentrated in vacuo. The residue was purified by flash chromatography (0-10% EtO Ac/heptane to afford the desired product 1 -(3 -bromo-4-methylphenyl)-2,5 -dimethyl- lH-pyrrole in 92% yield. LCMS (m/?) (M+H) = 265.8, Rt = 1.13 min.

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, 3-Bromo-4-methylaniline, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; NOVARTIS AG; AVERSA, Robert John; BURGER, Matthew T.; DILLON, Michael Patrick; DINEEN JR., Thomas A.; LOU, Yan; NISHIGUCHI, Gisele A; RAMURTHY, Savithri; RICO, Alice C.; RAUNIYAR, Vivek; SENDZIK, Martin; SUBRAMANIAN, Sharadha; SETTI, Lina Quattrocchio; TAFT, Benjamin R.; TANNER, Huw Rowland; WAN, Lifeng; (307 pag.)WO2016/38582; (2016); A1;,
Bromide – Wikipedia,
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Adding a certain compound to certain chemical reactions, such as: 876-53-9, name is 1,3-Dibromoadamantane, 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 876-53-9, 876-53-9

1. Under nitrogen protection, 440 g of 1,3-dibromoadamantane was added to a 10 L four-necked flask. Then 2.0 L of dichloroethane was added and stirred well, 500 g of acetanilide was added and stirred well. Add zinc dichloride slowly and stir it well, then heat up to reflux (internal temperature 80-85C). Partially separate the water with a water separator and then use a reflux device. After refluxing at this temperature for 24 hours, the lower layer was a viscous solid and the upper layer was a dichloroethane solvent. Cool to room temperature, pour off the upper layer of solvent, add 1.0L DMF (N,N-dimethylformamide) to raise the temperature to a solid slurry, and slowly pour the slurry into 4.0L of stirring water. Stir 30%. Filter after minutes The solid crude product was obtained in a wet weight of 1219 g. The solid was added to 6 L of water for beating for 3.5 hours, filtered and pumped until no liquid was dripped, and then washed with water (2¡Á2 L). 1332 g of crude wet weight was obtained, refluxed with two-fold volume of ethanol (3 L) for 1 hour, cooled to room temperature and stirred at room temperature for 1 hour, filtered to dry wet weight 522 g and used directly for the second reaction.

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, 1,3-Dibromoadamantane, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; Shanghai Bodong Chemical Technology Co., Ltd.; Fu Zhiwei; He Baoyuan; Pan Xingang; Yu Wenqing; Li Yongli; Lu Wei; (7 pag.)CN107673977; (2018); A;,
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1003-98-1, 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. 1003-98-1 name is 2-Bromo-4-fluoroaniline, 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.

2-Propyl-3-propyl-5-fluoro-1H-indole; A 50 mL three neck flask was charged with palladium acetate (22.4 mg, 0.1 mmol), dtbpf (94 mg, 0.2 mmol), potassium carbonate (690 mg, 5 mmol), 2-bromo-4-fluoroaniline (380 mg, 2 mmol), 4-octyne (264 mg, 2.4 mmol) and NMP (10 ml). The mixture was purged with argon and heated to 130 C. After 1 hr, the reaction mixture was cooled to rt. Ethyl acetate and water were added. The organic layer was separated and the aqueous layer was extracted with ethyl acetate. The combined organic phases were washed with water, brine and dried with MgSO4. Removal of the solvents and purification of the crude by column chromatography afforded the desired product as yellow oil (355 mg, containing 4.3 wt % AcOEt). The corrected yield was 77.6%. 1H NMR (400 MHz): delta=7.68 (s, 1H), 7.16-7.13 (m, 2H), 6.83 (td, 1H, J=9.2 Hz, J=2.4), 2.68 (t, 2H, J=7.6 Hz), 2.61 (t, 2H, J=7.6), 1.72-1.57 (m, 4H), 0.98 (t, 3H, J=7.2 Hz), 0.95 (t, 3H, J=7.2 Hz).

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; Boehringer Ingelheim International GmbH; US2005/209465; (2005); A1;,
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Some common heterocyclic compound, 40161-54-4, name is 1-Bromo-2-fluoro-4-(trifluoromethyl)benzene, 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. 40161-54-4

INTERMEDIATE 7 MC181 Y4-[2-Bromo-5-(trifluoromethyl)phenoxy]cvclohexanolTo a solution of 4-bromo-3-fluorobenzotrifluoride (2 g, 8.23 mmol) and a mixture of cis and trans cyclohexane-l,4-diol (3.82 g, 32.9 mmol) in DMF (41.2 ml) was added NaH 5 (0.658 g, 16.46 mmol) at 0 C. The reaction mixture was warmed to room temperature then heated at 80 0C for 2 h. The mixture was poured onto IN HCl (100 mL) and extracted with EtOAc (3×25 mL). The combined organic fractions were washed with water (50 mL) then dried over Na2SO4. Purification by Combiflash chromatography (SiO2-40 g, gradient elution of 10- 50% EtOAc/hexanes over 25 min) afforded the title product as a 7:3 mixture of isomers. 10 Major isomer: 1H NMR (500 MHz, acetone-d6): delta 7.82 (dd, IH), 7.43 (d, IH), 7.23 (d, IH), 4.76-4.70 (m, IH), 3.84-3.76 (m, IH), 3.67 (d, IH), 2.18-2.12 (m, IH), 2.06-1.95 (m, IH), 1.82-1.71 (m, 2H), 1.69-1.60 (m, 2H), 1.55-1.47 (m, 2H). MS: m/z 339, 341 (MH+).

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 40161-54-4, its application will become more common.

Reference:
Patent; MERCK FROSST CANADA LTD.; WO2008/128335; (2008); A1;,
Bromide – Wikipedia,
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The chemical industry reduces the impact on the environment during synthesis 142808-15-9, name is 4-Bromo-2-fluorobenzotrifluoride, I believe this compound will play a more active role in future production and life. 142808-15-9

At -78 C., 181.07 ml of a 2.5M (452.7 mmol) solution of n-butyllithium were added dropwise to a solution of 63.9 g (452.7 mmol) of 2,2,6,6-tetramethylpiperidine in 833 ml of dry THF. The mixture was stirred at this temperature for 30 min. 100.0 g (411.5 mmol) of 4-bromo-2-fluoro-1-(trifluoromethyl)benzene were then added dropwise at -78 C. The mixture was stirred at this temperature for 2 h. 33.1 g (452.7 mmol) of DMF were then added dropwise at -78 C. The reaction mixture was then stirred for 2 h. For work-up, 300 ml of water were added to the contents. The mixture was extracted three times with in each case 200 ml of dichloromethane. The combined organic phases were washed with 300 ml of 1M hydrochloric acid and then with 300 ml of a saturated aqueous sodium chloride solution. The organic phase was dried and the filtrate was freed of the solvent. 96.2 g of the desired product were obtained.

The chemical industry reduces the impact on the environment during synthesis 142808-15-9. I believe this compound will play a more active role in future production and life.

Reference:
Patent; BAYER CROPSCIENCE AKTIENGESELLSCHAFT; AHRENS, Hartmut; TIEBES, Joerg; WALDRAFF, Christian; DIETRICH, Hansjoerg; SCHMUTZLER, Dirk; GATZWEILER, Elmar; ROSINGER, Christopher; (33 pag.)US2017/107183; (2017); A1;,
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39478-78-9, 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. 39478-78-9, name is 5-Bromo-2-methylaniline belongs to bromides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

5-Bromo-2-methylphenol; A solution of concentrated sulphuric acid (6 mL) in distilled water (75 mL) was added to 5-bromo-2-methylaniline (1 g, 5.38 mmol). The resultant suspension was heated to 90 C. and stirred for 4.5 h. The reaction mixture was then cooled using an ice bath and a solution of sodium nitrite (384 mg, 5.57 mmol) in water (5 mL) was added to the reaction mixture at 0 C. The reaction was then allowed to warm to ambient temperature. The reaction mixture was then added to a solution of concentrated sulphuric acid (6 mL) in water (75 mL) which had been preheated to 90 C. The reaction mixture was stirred for 1 h at 90 C. and allowed to cool, on standing, overnight. A precipitate was observed in the reaction mixture. The precipitate was collected by filtration, washed with water, and dried in a vacuum oven to afford 5-bromo-2-methylphenol as a brown solid (510 mg, 2.73 mmol, 51%). M.S. (ESI) (m/z) 185, 187[M-H]-

The synthetic route of 39478-78-9 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; N.V. Organon; US2007/185156; (2007); A1;,
Bromide – Wikipedia,
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22385-77-9, 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. 22385-77-9, name is 1-Bromo-3,5-di-tert-butylbenzene, This compound has unique chemical properties. The synthetic route is as follows.

2-methyl-4-methoxy-7-(3,5-Di-tert-butylphenyl)-1H-indene To a solution of 3,5-di-tert-butylphenylmagnesium bromide obtained from 59.3 g (0.220 mol) of 1-bromo-3,5-di-tert-butylbenzene and 7.60 g (0.313 mol, 1.42 eqv.) of magnesium turnings in 450 ml of THF 1.00 g (1.28 mmol, 0.65 mol. percent) NiCl2(PPh3)IPr and a solution of 53.4 g (0.197 mol) of 2-methyl-4-bromo-1,7-dimethoxyindane in 50 ml of THF were added. A vigorous reflux occurs approximately after ca. 30 sec and ceased after the following 30 sec. This mixture was stirred for 30 min at room temperature. Finally, 1000 ml of water and then 50 ml of 12 M HCl were added. The product was extracted with 500 ml of dichloromethane, organic layer was separated, the aqueous layer was additionally extracted with 200 ml of dichloromethane. The combined organic extract was dried over K2CO3, passed through a short column with silica gel 60 (40-63 mum), and then evaporated to dryness. To the residue dissolved in 700 ml of toluene 1.4 g of TsOH was added. This solution was refluxed using Dean-Stark head for 20 min, cooled to room temperature, washed with 200 ml of 10percent aqueous NaHCO3. The organic layer was separated, the aqueous layer was extracted with 2*100 ml of dichloromethane. The combined organic solution was evaporated to dryness. The product was isolated by flash chromatography on silica gel 60 (40-63 um; eluent: hexane-dichloromethane=10:1, then 1:1, vol.). This procedure gave 67.6 g (99percent) of 2-methyl-4-methoxy-7-(3,5-di-tert-butylphenyl)-1H-indene as a yellowish crystalline powder. The latter can be recrystallized from n-hexane with marginal loss of weight. Anal. calc. for C25H32O: C, 86.15; H, 9.25. Found: C, 86.09; H, 9.23. 1H NMR (CDCl3): delta 7.40 (m, 1H, 4-H in tBu2C6H3), 7.35 (m, 2H, 2,6-H in tBu2C6H3), 7.15 (d, J=8.4 Hz, 1H, 6-H in indenyl), 6.88 (d, J=8.4 Hz, 1H, 5-H in indenyl), 6.70 (m, 1H, 3-H in indenyl), 3.92 (s, 3H, OMe), 3.41 (m, 2H, 2,2′-H in indenyl), 2.15 (s, 3H, 2-Me in indenyl), 1.38 (s, 18H, tBu).

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; BOREALIS AG; RESCONI, Luigi; CASTRO, Pascal; VIRKKUNEN, Ville; IZMER, Vyatcheslav V.; KONONOVICH, Dmitry S.; KULYABIN, Pavel Sergeevich; VOSKOBOYNIKOV, Alexander Z.; US2015/344596; (2015); A1;,
Bromide – Wikipedia,
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A common compound: 3638-73-1, name is 2,5-Dibromoaniline, belongs to bromides-buliding-blocks compound, it can change the direction of chemical reaction, and react with certain compounds to generate new functional products. A new synthetic method of this compound is introduced below. 3638-73-1

General procedure: To a mixture of 2-naphthol (1 mmol), aniline derivatives(1 mmol) and Kojic aldehyde (1 mmol) was added nanoFe3O4(at)SiO2-boric acid (15 mg). The mixture was stirredat 40 C under solvent free condition in an oil bath and thecompletion of reaction was monitored by TLC (EtOAc / nhexane:1:4). After completion of the reaction, the mixturewas cooled to room temperature, ethanol (2 mL) was added,and themixture was stirred for 10 min. The catalyst was separatedout using an external magnet and the obtained solid wascollected by filtration and purified by recrystallization from(EtOH/acetone, 4:1) or was subjected to silica gel preparativelayer chromatography (EtOAc/n-hexane, 1:5) to give pyran asa pure solid. The recovered catalyst was washed with EtOH,dried and reused for the next run. The catalyst was recoveredand reused for five times without any significant changes inthe yield and the reaction time.

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, 3638-73-1, other downstream synthetic routes, hurry up and to see.

Reference:
Article; Teimuri-Mofrad, Reza; Gholamhosseini-Nazari, Mahdi; Esmati, Somayeh; Shahrisa, Aziz; Journal of Chemical Sciences; vol. 129; 9; (2017); p. 1449 – 1459;,
Bromide – Wikipedia,
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1435-51-4, 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 1435-51-4 as follows.

step 1-A solution of 57a, sodium methoxide (1 equivalent) and DMF were stirred overnight under an N2 atmosphere at RT. The volatile solvents were removed in vacuo and the residue partitioned between Et2O and water. The organic phase was washed with 5% NaOH, water and brine, dried (MgSO4), filtered and evaporated to afford 57b.

According to the analysis of related databases, 1,3-Dibromo-5-fluorobenzene, the application of this compound in the production field has become more and more popular.

Reference:
Patent; Roche Palo Alto LLC; US2006/25462; (2006); A1;,
Bromide – Wikipedia,
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The chemical industry reduces the impact on the environment during synthesis 38573-88-5, name is 1-Bromo-2,3-difluorobenzene, I believe this compound will play a more active role in future production and life. 38573-88-5

Preparation 8; TERT-BUTYL S-^1S-DIFLUOROPHENYL)-S-HYDROXYAZETIDINE-I – CARBOXYLATE; To a solution of 3-bromo-1 ,2-difluorobenzene (2.3 g, 11.8 mmol) in dry diethylether (20 ml) at -78¡ãC, under nitrogen was added n-butyllithium (2.5 M in hexane, 4.7 ml, 11.8 mmol) dropwise. The mixture was stirred for 1 h after which a solution of 1-Boc-3-azetidinone (2.0 g, 11.7 mmol) in dry diethyl ether (20 mL) was added dropwise. The resulting mixture was stirred at -78¡ãC for 15 min and then brought to ambient temperature and stirred for 2 h. Aqueous ammonium chloride (50 mL, 50percent) and diethylether was added, the organic phase was collected and the aqueous phase was extracted with ethyl acetate (2×50 ml). The combined organic phase was dried (Na2SO4), filtered and evaporated to dryness. The crude product was purified by flash column chromatography on silica gel (ethylacetate/isooctane 1 :4 to 1 : 1 ) to give the title compound (1.9 g). MS m/z (rel. intensity, 70 eV) 285 (M+, 1 ), 156 (55), 141 (69), 127 (bp), 57 (88).

The chemical industry reduces the impact on the environment during synthesis 38573-88-5. I believe this compound will play a more active role in future production and life.

Reference:
Patent; NSAB, FILIAL AF NEUROSEARCH SWEDEN AB, SVERIGE; SONESSON, Clas; SWANSON, Lars; PETTERSSON, Fredrik; WO2010/58017; (2010); A1;,
Bromide – Wikipedia,
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