Month: January 2021

Related Products of 858121-94-5, 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. 858121-94-5, name is 4-(Bromomethyl)-1,1-difluorocyclohexane belongs to bromides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

To a solution of 4-(bromomethyl)-1 ,1-difluorocyclohexane (600 mg, 0.0028 mol, Intermediate 3) in Lambda/,/V-dimethylformamide (6 mL), sodium azide (549 mg, 0.0084 mol) was added at 26 C. The reaction mixture was heated to 100 C and stirred for 16 h at the same temperature. Upon completion, the reaction mixture was used for the next step without any further purification.1H NMR (400 MHz, CDCI3) 53.18 (t, J = 6.6 Hz, 2H), 2.17-1.98 (m, 2H), 1.85-1.57 (m, 5H), 1.37- 1.20 (m, 2H).

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-(Bromomethyl)-1,1-difluorocyclohexane, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; GLAXOSMITHKLINE INTELLECTUAL PROPERTY DEVELOPMENT LIMITED; ALEMPARTE-GALLARDO, Carlos; ENCINAS, Lourdes; ESQUIVIAS PROVENCIO, Jorge; (206 pag.)WO2019/34729; (2019); A1;,
Bromide – Wikipedia,
bromide – Wiktionary

Adding a certain compound to certain chemical reactions, such as: 6274-57-3, name is 1-(4-Bromophenyl)-N,N-dimethylmethanamine, 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 6274-57-3, name: 1-(4-Bromophenyl)-N,N-dimethylmethanamine

Example 39 Preparation of Compound 73 (0279) (0280) To 4?-bromobenzyldiethylamine (0.3 g, 1.23 mmol) in anhydrous THF (10 mL) at -78 C. under N2 was added 2.5 M n-butyllithium in hexanes (0.5 mL, 1.23 mmol) and then followed by the addition of 1,2-dihydro-4-methyl-1-phenyl-2-quinolone (0.3 g, 1.25 mmol) in THF (10 mL). The mixture was stirred at -78 C. for 1 hour and HOAc (0.5 mL) was added. The mixture was stirred at room temperature for another hour and then concentrated to dryness in vacuo. The residue was dissolved in CH2Cl2 (10 mL) and then followed by the addition of 1-(methylthio)-7,8-dihydro-6H-thiazolo[5,4,3-ij]quinolin-9-ium tosylate (0.484 g, 1.23 mmol) and triethylamine (0.56 mL). The mixture was stirred at room temperature for 2 hrs and concentrated to dryness in vacuo. The residue was dissolved in MeOH (5 mL) and then added dropwise to a solution of NaI (2 g) in water (50 mL). The orange precipitate (42 mg) was collected by suction filtration and dried to a constant weight.

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; BIOTIUM, INC.; Mao, Fei; Cheung, Chingying; Leung, Wal-Yee; Windler, Sarah Lynn; Roberts, Lori M.; (76 pag.)US2016/24067; (2016); A1;,
Bromide – Wikipedia,
bromide – Wiktionary

Related Products of 4117-09-3, 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 4117-09-3 as follows.

General procedure: To 35.2 mL of 1,3-diaminopropane (422 mmol) at 0 C and under argon was added dropwise 5-bromopent-1-ene (5.0 mL, 42.2 mmol). The solution was stirred at 0 C one hour, and two additional hours at room temperature. The reaction mixture was then partitioned between AcOEt (250 mL), brine (40 mL), saturated aqueous NaHCO3 (40 mL), and H2O (40 mL). The aqueous layer was extracted with AcOEt and the combined organic extracts were dried over Na2SO4, filtered, and concentrated in vacuo. Purification by flash column chromatography on SiO2 with CHCl3/MeOH/NH4OH gradients afforded pure alkyl diamine 1 (5.64 g, 94%)

According to the analysis of related databases, 4117-09-3, the application of this compound in the production field has become more and more popular.

Reference:
Article; Decroos, Christophe; Bowman, Christine M.; Christianson, David W.; Bioorganic and Medicinal Chemistry; vol. 21; 15; (2013); p. 4530 – 4540;,
Bromide – Wikipedia,
bromide – Wiktionary

Adding a certain compound to certain chemical reactions, such as: 444-14-4, name is 2-Bromo-4,6-difluoroaniline, 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 444-14-4, HPLC of Formula: C6H4BrF2N

Commercially available bromodifluoroaniline (11) is treated with di-tert-butyldicarbonate to give protected aniline 12. Alkylation of aniline 12 gives the N-ethyl derivative 13, which is converted to the lithium derivative by metal halogen exchange, and added to the Boc-protected aziridine 3a under copper catalysis, yielding intermediate 14. The acetal protecting group is removed and the resulting diol 15 is converted to epoxide 16 using well-known procedures.

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; ELAN PHARMACEUTICALS, INC.; WO2005/87752; (2005); A2;,
Bromide – Wikipedia,
bromide – Wiktionary

Synthetic Route of 22385-77-9, The chemical industry reduces the impact on the environment during synthesis 22385-77-9, name is 1-Bromo-3,5-di-tert-butylbenzene, I believe this compound will play a more active role in future production and life.

1-Bromo-3,5-tert-butylbenzene (2.50 equivalents, CAS: 22385-77-9) in dry THF is added dropwise to activated magnesium turnings suspended in dry THF under N2 atmosphere. After addition, the mixture is refluxed for a few hours until 1-bromo-3,5-tert-butylbenzene (CAS: 22385-77-9) is consumed completely and the mixture becomes dark brown. The resulting Grignard reagent is slowly added to cyanuric chloride (1.00 equivalent in dry toluene, CAS: 108-77-0) at room temperature (RT) (the cyanuric chloride was previously prepared in another flask). After addition, the mixture is refluxed overnight and cooled to RT. The crude product 2- chloro-4,6-bis(3,5-di-tert-butylphenyl)-1 ,3,5-triazine is extracted with DCM/brine and recrystallized from EtOH/DCM (20:1 ) to yield 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-Bromo-3,5-di-tert-butylbenzene, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; CYNORA GMBH; SZAFRANOWSKA, Barbara; PINGEL, Patrick; BERGMANN, Larissa; AMBROSEK, David; KASPAREK, Christian; (0 pag.)WO2019/162332; (2019); A1;,
Bromide – Wikipedia,
bromide – Wiktionary

Synthetic Route of 2255-80-3,Some common heterocyclic compound, 2255-80-3, name is 4-Bromo-7-methylbenzo[c][1,2,5]thiadiazole, molecular formula is C7H5BrN2S, 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.

4-Bromo-7-methylbenzo[c][l,2,5]thiadiazole (0.25 g, 1.1 mmol) was dissolved in AcOH (12 ml) and H2SO4 (1.7 ml). [CAUTION: Exothermic]. The solution was then treated with chromium (VI) oxide (1.5 g) portionwise and stirred for 30 mins. The reaction was then poured onto ice and allowed to warm to room temperature. The aqueous layer was then extracted with DCM (3 x 30 ml). The aqueous layer was left overnight and the precipitate filtered and washed with water (3 x 2 ml) to afford the title compound as a white solid (0.085 g, 30 %); vmax(thin film) 3100 – 3300 (broad – OH), 1682 (C=O), 1680, 1525, 1312, 1289, 1193 cm-1; deltaH(500 MHz, (CD3)2CO) 8.31 (IH, d, / 8, Ar-H), 8.15 (1eta, d, / 8, Ar-H), 2.09 (1eta, s, CO2H); deltaC (126 MHz, (CDs)2CO) 165.1 (C=O), 154.8 (C=N), 152.6 (C=N), 134.7 (Ar-C), 132.6 (Ar-Q, 124.2 (ipso-Ar-Q, 120.1 (ipso-Ai-Q; m/z (ES”) 259 ([81Br]M”), 257 ([79Br]M”); HRMS (ES”) Found M”, 256.90248 (C7H279BrN2O2S requires 256.90258).

The synthetic route of 2255-80-3 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; UNIVERSITY OF DURHAM; WO2009/34396; (2009); A2;,
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. 314084-61-2, name is 2-Bromo-1,3-diethyl-5-methylbenzene, A new synthetic method of this compound is introduced below., Application In Synthesis of 2-Bromo-1,3-diethyl-5-methylbenzene

Into an oven-dried 35 ml_ carousel reaction tube fitted with a magnetic stirrer bar was added the palladium source, APhos (4-di-ferf-butylphoshanyl-N,N-dimethyl-aniline, 0 – 20 mol%), 1 ,2,4,5- tetrahydropyrazolo[1 ,2-d][1 ,4,5]oxadiazepine-7,9-dione (1.2 equiv.) and K3PO4 (2.1 equiv.) under an atmosphere of N2 gas. A solution of 2-bromo-1 ,3-diethyl-5-methyl-benzene (DEMBB, 1 equiv.) and mesitylene (0.25 equiv. as an internal standard) in 1 ,4-dioxane (1 – 3 ml) was purged of oxygen by bubbling with N2 gas for 20 mins and then transferred to the reaction tube which was then placed immediately into the pre-heated carousel at 1 10 C and stirred for 6 h. Sampling procedure: A small aliquot of the reaction mixture was quenched with HCI (aq, 1 M) and extracted into EtOAc. The conversion was determined by NMR spectroscopy and/or GC analysis against mesitylene as an internal standard, or 1 , 3, 5-trimethoxybenzene as an external standard. The above general procedure (example 3) was used to obtain the results referred to in Table 2 below. (0136) Table 2 – Summary of results comparing differing palladium catalysts with the APhos ligand

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; SYNGENTA PARTICIPATIONS AG; MORRIS, James, Alan; SALE, David, Alexander; SHAFIR, Alexandr; GONU, Mallikharjuna; BILAL, Iffat; (27 pag.)WO2019/110613; (2019); A1;,
Bromide – Wikipedia,
bromide – Wiktionary

Adding a certain compound to certain chemical reactions, such as: 6911-87-1, name is 4-Bromo-N-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 6911-87-1, Recommanded Product: 6911-87-1

General procedure: A 25 mL oven-dried Schlenk tube was sequentially added N-methylaniline 1 or aniline 4 (0.2 mmol), Ethyl Bromodifluoroacetate 2a (81.2 mg, 0.4 mmol), DMF (1ml) and H2O (1 mL) was added under air. The reaction mixture was stirred for 6 h at 110. The solution was then diluted with ethyl acetate (20 mL), washed with brine (10 mL), extracted with ethyl acetate (3*5 mL), dried over anhydrous Na2SO4, filtered and evaporated under vacuum. The crude reaction mixture was purified by column chromatography (silica gel, ethyl acetate/petroleum ether) yielded the desired product 3 or 5.

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

Reference:
Article; Xu, Zhuo-Wei; Xu, Wen-Yi; Pei, Xiao-Jun; Tang, Fei; Feng, Yi-Si; Tetrahedron Letters; vol. 60; 18; (2019); p. 1254 – 1258;,
Bromide – Wikipedia,
bromide – Wiktionary

Electric Literature of 6627-78-7, 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. 6627-78-7 name is 1-Bromo-4-methylnaphthalene, 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.

A 5 L four-necked flask was charged with 461.8 g of 4-bromo-1-methylnaphthalene (I)7.2kg of carbon tetrachloride,375.6 g of N-bromosuccinimide,20.5 g BP0,The temperature was raised to 70 to 78 C (preferably 77 C) and the reaction was refluxed overnight.Point plate,The reaction is complete.Cooled to room temperature,Filter,40 C spin dry solvent.Add 1200 g of ethanol,Heating up to 70 C Paul lh,Cooling to room temperature,Filter,Filter cake washed with ethanol,After draining,Dried at 35 C to give 500 g of 4-bromo-1-bromomethylnaphthalene (II)The two-step yield was 79% (based on 1-methylnaphthalene).

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

Reference:
Patent; Shanghai Ya Ben Chemical Co., Ltd.; Zhou, Yu; Xiao, Fangliang; Shi, Wei; Xu, Meng; (7 pag.)CN106366018; (2017); A;,
Bromide – Wikipedia,
bromide – Wiktionary

Application of 16518-62-0, 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. 16518-62-0 name is 3-Bromo-N,N-dimethylaniline, 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.

EXAMPLE 2 Preparation of 1-(4-chlorobenzyl)-3-dimethyl-amino-6-(3-fluoro-4-isopropoxyphenylamino)benzene (I-123) To a mixture of 3-bromo-1-dimethyl-aminobenzene (0.3 g, 1.5 mmol) and THF (3 mL) were added 4-chlorobenzyl zinc chloride (0.5 M THF solution, 6 mL, 3 mmol), triphenylphosphine (39.3 mg, 0.15 mmol) and palladium acetate (II) (17 mg, 0.08 mmol), and the resulting mixture was heated at reflux for 2 hours. To the reaction mixture was added water (200 mL), and the resulting mixture was extracted with ethyl acetate (200 mL). The extract was washed by brine (100 mL), dried over anhydrous magnesium sulfate, and concentrated in vacuo. The resulting residue was purified by silica gel column chromatography (ethyl acetate/hexane) to give 1-(4-chlorobenzyl-3-dimethyl-aminobenzene (0.32 g, Yield: 87percent) as colorless oil. 1H-NMR, (delta ppm TMS/CDCl3): 2.89 (6H, s), 3.87 (2H, s), 6.48-6.59 (4H, m), 7.08-7.22 (4H, m).

At the same time, in my other blogs, there are other synthetic methods of this type of compound, 3-Bromo-N,N-dimethylaniline, and friends who are interested can also refer to it.

Reference:
Patent; SHIONOGI & CO., LTD.; Kai, Hiroyuki; Endoh, Takeshi; Jikihara, Sae; Horiguchi, Tohru; US9212130; (2015); B2;,
Bromide – Wikipedia,
bromide – Wiktionary