Month: February 2021

Related Products of 698-00-0, 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. 698-00-0, name is 2-Bromo-N,N-dimethylaniline belongs to bromides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

Example 1512-{4-[4-(2-methoxyphenyl)piperazin- I -yI]-1 H-pyrazolo[3,4-d]pyrimidin- I -yI}-N,Ndimethylaniline 80 mg (0.26 mmo[) 4-[4-(2-methoxypheny[)piperazin-1 -y[]-1 H-pyrazo[o[3,4-d]pyrimidine, 77.4 mg (0.39 mmo[) 2-bromo-N,N-dimethy[ani[ine, 14.7 mg (0.08mmo[) copper(I) iodide, 115 mg (0.54 mmo[) tripotassium phosphate and 22mg (0.16mmo[) trans-N,N?-dimethy[cyc[ohexane-1,2-diamine in 3 mL anhydrous NMP wereheated under microwave irradiation at 180CC for 8 h. The reaction mixture waspoured into water and extracted three times with ethy[ acetate. The combinedorganic phases were washed with 0.5 M aqueous EDTA so[ution and three times with water, dried over magnesium su[fate and concentrated. The residue was purified by HPLC affording 3 mg (3%) product.LC-MS (ana[ytica[ method 3): R = 1 .09 mm, MS (ESipos): mlz = 430 (M+H).1H-NMR (300MHz, CHLOROFORM-d): 6 [ppm]= 2.52 (5, 6H), 3.25 – 3.33 (m, 4H), 3.96 (5, 3H), 4.22 – 4.30 (m, 4H), 6.92 – 7.16 (m, 6H), 7.31 (d, 1H), 7.36 – 7.45 (m, 1H), 8.25 (5, 1H), 8.45 (5, 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-N,N-dimethylaniline, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; BAYER PHARMA AKTIENGESELLSCHAFT; HEISLER, Iring; MUeLLER, Thomas; GOLZ, Stefan; TELSER, Joachim; REHWINKEL, Hartmut; SIEBENEICHER, Holger; BUCHMANN, Bernd; ZORN, Ludwig; EIS, Knut; KOPPITZ, Marcus; LINDNER, Niels; HEROULT, Melanie; NEUHAUS, Roland; WO2013/182612; (2013); A1;,
Bromide – Wikipedia,
bromide – Wiktionary

Application of 3814-30-0, The chemical industry reduces the impact on the environment during synthesis 3814-30-0, name is (Bromomethyl)cyclopentane, I believe this compound will play a more active role in future production and life.

General procedure: To a stirred solution of ethyl 2-(4-aminophenoxy)-2-methylpropanoate 12 (1 equiv) and anhydrous potassium carbonate(0.5 equiv) in dry DMF was slowly added the corresponding alkyl bromides (1 equiv), and then heated to 80 C until the reaction completed. The mixture was added ethyl acetate and washed with water and brine successively, dried, filtered and concentrated under reduced pressure. The residue was purified by column chromatography.

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, (Bromomethyl)cyclopentane, other downstream synthetic routes, hurry up and to see.

Reference:
Article; Li, Yongqiang; Tian, Kang; Qin, Aifang; Zhang, Lijian; Huo, Lianchao; Lei, Lei; Shen, Zhufang; Song, Hongrui; Feng, Zhiqiang; European Journal of Medicinal Chemistry; vol. 76; (2014); p. 182 – 192;,
Bromide – Wikipedia,
bromide – Wiktionary

Electric Literature of 583-70-0, The chemical industry reduces the impact on the environment during synthesis 583-70-0, name is 2,4-Dimethylbromobenzene, I believe this compound will play a more active role in future production and life.

(Diethylamino)-bis(2,4-dimethylphenyl)phosphine (B46): A solution of 2.92 ml (21.61 mmol) of 4-bromo-1,3-dimethylbenzene in 3 ml of Et2O were added at 0 C. to a suspension of 0.5 g (20.56 mmol) of magnesium turnings in 7 ml of THF and 7 ml of Et2O and also a crystal of iodine. The mixture was heated to room temperature, stirred further overnight and slowly added dropwise at 0 C. to a solution of 1.5 ml (10.31 mmol) of Et2NPCl2 in 8 ml of THF. The mixture was heated to 5-10 C., stirred for a further 2 hours and the solvent was subsequently removed under reduced pressure. After adding 60 ml of hexane, the mixture was filtered through Celite under argon and the solvent was subsequently removed under reduced pressure. Yield: 1.37 g (59% of theory). 1H NMR (400 MHz, CDCl3) delta, 6.9 (m, 6H), 3.03 (m, 4H, CH2), 2.20 (s, 12H, CH3), 0.81 (t, 3J=7.0 Hz, 6H, CH3) 31P NMR (161.9 MHz, CDCl3) delta, 47.8.

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, 2,4-Dimethylbromobenzene, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; Meseguer, Benjamin; Militzer, Hans-Christian; Castillon, Sergio; Claver, Carmen; Diaz, Yolanda; Aghmiz, Mohamed; Guiu, Ester; Aghmiz, Ali; Masdeu, Anna; US2005/80047; (2005); A1;,
Bromide – Wikipedia,
bromide – Wiktionary

Related Products of 1195-33-1, 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 1195-33-1 as follows.

General procedure: A sealable reaction tube equipped with a magnetic stirrer bar was charged with 2-(allyloxy)benzaldehyde (0.2mmol), benzenesulfinic acid (3.0 equiv.), Na2-Eosin Y (4 mol%), K2S2O8 (3.0 equiv.), DMF_H2O=1:1 (2 ml), 8W blue. The reaction vessel was carried out room temperature. After completion, it was diluted with ethylacetate, washed with water. After the solvent was removed under reduced pressure, the residue was purified bycolumn chromatography on silica gel to afford the corresponding product.

According to the analysis of related databases, 1195-33-1, the application of this compound in the production field has become more and more popular.

Reference:
Article; Chen, De-Mao; Han, Qing-Qing; Li, Guang-Hui; Sun, Yuan-Yuan; Wang, Zu-Li; Xu, Xin-Ming; Yu, Xian-Yong; Chinese Chemical Letters; (2020);,
Bromide – Wikipedia,
bromide – Wiktionary

Application of 6274-57-3, 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. 6274-57-3 name is 1-(4-Bromophenyl)-N,N-dimethylmethanamine, 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.

General procedure: At room temperature, organic carbonyl acid 3 (R-COOH, 0.5 mmol) was added into a reaction tube equipped with a small magnet. Then a solution of tertiary amine 1 (R1CH2-NR2R3, 0.5 mmol ) in DCM (2.5 mL) was added dropwise in 2 min. After the mixture was stirred at room temperature for a few minutes, 1 equivalents of dimethyl acetylenedicarboxylate (DMAD, 2) was added. The reaction was stirred overnight at room temperature, and then monitored by TLC with silica gel coated plates. After being stirred for 14 h, the solvent was removed and the residue was purified by a flash column chromatography with silica gel with ethyl acetate/hexane (1:25-30) as eluent to give the desired products 4, 5, and 7. Most of compounds are known and confirmed by NMR, ESI-MS, IR.

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

Reference:
Article; Shen, Hao; Lu, Xing; Jiang, Ke-Zhi; Yang, Ke-Fang; Lu, Yixin; Zheng, Zhan-Jiang; Lai, Guo-Qiao; Xu, Li-Wen; Tetrahedron; vol. 68; 43; (2012); p. 8916 – 8923;,
Bromide – Wikipedia,
bromide – Wiktionary

Synthetic Route of 3972-64-3, A common heterocyclic compound, 3972-64-3, name is 1-Bromo-3-(tert-butyl)benzene, molecular formula is C10H13Br, 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.

2-(3-(Tert-butyl)phenyl)ethanol To a vial was added the 1-bromo-3-(tert-butyl)benzene (0.107 g, 0.502 mmol) and dry THF. The reaction was then cooled to -78¡ã C. and the BuLi (0.221 mL, 0.552 mmol) (2.5 M in hexanes) was added dropwise and the reaction stirred for 30 min at -78¡ã C. and then ethylene oxide (0.502 mL, 1.255 mmol) (2.5-3.3M solution in THF) was added dropwise and the reaction stirred for 10 minutes at -78¡ã C. then warmed to rt and stirred for 1 h. The reaction was then quenched with 1.0 M HCl (2 mL) and extracted with EtOAc (3*5 mL). The EtOAc layer was combined, concentrated and purified by reverse-phase MPLC (10-100percent MeCN:water) to produce pure 2-(3-(tert-butyl)phenyl)ethanol (0.035 g, 0.196 mmol, 39percent yield). 1H NMR (400 MHz, CDCl3): delta 7.31-7.27 (m, 3H), 7.10-7.07 (m, 1H), 3.90 (t, J=6.6 Hz, 2H), 2.91 (t, J=6.5 Hz, 2H), 1.52 (br s, 1H), 1.36 (s, 9H).

The synthetic route of 3972-64-3 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; UNIVERSITY OF ROCHESTER; UNIVERSITY OF KANSAS; Dunman, Paul M.; Krysan, Damian J.; Flaherty, Daniel P.; US2015/238473; (2015); A1;,
Bromide – Wikipedia,
bromide – Wiktionary

These common heterocyclic compound, 2550-36-9, name is (Bromomethyl)cyclohexane, 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. category: bromides-buliding-blocks

1H-indole-6-carboxylic acid methyl ester (300mg, 1.71mmol) was dissolved in dimethyl formamide (7ml). Bromomethyl cyclohexane (0.5ml, 3.42mmol) and sodium hydride (150mg, 3.42mmol) were added dropwise thereto at 0, and then the mixture was stirred for 8 hours at room temperature. 1N hydrochloric acid solution was added, and the mixture was extracted with ethyl acetate. The extract was washed with saturated aqueous sodium chloride solution, dried over anhydrous magnesium sulfate and filtered. Filtrate was distilled under reduced pressure and separated by column chromatography to obtain the title compound (150mg, 32%). [611] NMR:1H-NMR(400HMz, CDCl3); delta 7.29-7.39 (m, 2H), 7.19 (d, 1H), 7.13 (m, 1H), 7.00-7.09 (m, 2H), 6.66 (m, 1H), 4.83 (s, 2H), 2.06 (s, 3H)

The synthetic route of (Bromomethyl)cyclohexane has been constantly updated, and we look forward to future research findings.

Reference:
Patent; LG LIFE SCIENCES LTD.; LEE, Sung Bae; PAEK, Seung Yup; YOON, Sook Kyung; YOON, Seung Hyun; CHOI, Jeung Soon; WO2014/73904; (2014); A1;,
Bromide – Wikipedia,
bromide – Wiktionary

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. 49764-63-8, name is 4,5-Dibromobenzene-1,2-diamine, This compound has unique chemical properties. The synthetic route is as follows., COA of Formula: C6H6Br2N2

To a solution of methyl (S)-4-(2-(2-formylbenzoyl)-5,5,8a-trimethyl-1,2,3,5,8,8a- hexahydroisoquinolin-6-yl)benzoate (50 mg, 0.113 mmol) and 4,5-dibromobenzene-1,2- diamine (30 mg, 0.113 mmol) in DMF (2 ml) was added sodium metabisulfite (24 mg, 0.124 mmol). The mixture was stirred at 60 C overnight. The mixture was concentrated in vacuo. The residue was partitioned between EtOAc (20 ml) and H2O (20 ml). The separated aqueous layer was extracted with EtOAc (20 ml). The combined organic layers were washed brine (20 ml), dried over Na2S04, and concentrated in vacuo. The crude product was purified by silica gel column eluted with 35 % EtOAc / hexanes to give the desired product (62 mg, 80 %) as a solid. LC/MS m/z 688.10 (M+H)+, 2.91 min (Method 2).

Chemical properties determine the actual use. Each compound has specific chemical properties and uses. We look forward to more synthetic routes in the future to expand reaction routes of 49764-63-8.

Reference:
Patent; VIIV HEALTHCARE UK (NO.5) LIMITED; CHEN, Jie; MEANWELL, Nicholas A.; REGUEIRO-REN, Alicia; SIT, Sing-Yuen; SWIDORSKI, Jacob; (267 pag.)WO2018/2848; (2018); 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. 103273-01-4, name is 2-Bromo-4-(tert-butyl)aniline, A new synthetic method of this compound is introduced below., Application In Synthesis of 2-Bromo-4-(tert-butyl)aniline

2-Bromo-4-tert-butyl-phenylamine (162 g, 0.71 mol) was added dropwise to H2SO4 (410 mL) at room temperature to yield a clear solution. This clear solution was then cooled down to -5 to -10 C. A solution of KNO3 (82.5 g, 0.82 mol) in H2SO4 (410 mL) was added dropwise while the temperature was maintained between -5 to -10 C. Upon completion, the reaction mixture was poured into ice/water and extracted with EtOAc. The combined organic layers were washed with 5% Na2CO3 and brine, dried over Na2SO4 and concentrated. The residue was purified by a column chromatography (EtOAc/petroleum ether 1/10) to give 2-bromo-4-tert-butyl-5-nitro-phenylamine as a yellow solid (152 g, 78%).

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; Vertex Pharmaceuticals Incorporated; US2012/309758; (2012); A1;,
Bromide – Wikipedia,
bromide – Wiktionary

Reference of 7073-94-1, 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. 7073-94-1 name is 1-Bromo-2-isopropylbenzene, 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.

Add 4.8 mmol (117 mg) of magnesium metal to a 25 mL Shrek bottle, 10 mL of tetrahydrofuran and 4 mmol (0.62 mL) of 2-isopropylbromobenzene, Stir at room temperature for 1h, Let stand. In a 250 mL three-necked flask, add 0.4 mmol (232 mg) of the compound represented by formula (XIa) and 80 mL of tetrahydrofuran. Cool to -20 , The fresh Grignard reagent was transferred to a 25 mL constant pressure dropping funnel and slowly added to the reaction system. After the dropping was completed, the system was transferred to room temperature and the reaction was continued for 12 h. After the reaction was completed, a saturated ammonium chloride solution was added to quench it. Extract the aqueous phase with ethyl acetate, The organic phases were combined, washed with a saturated sodium chloride solution and dried over anhydrous sodium sulfate. The solvent was spin-dried column chromatography (silica gel 100-200 mesh, eluent: dichloromethane / ethyl acetate = 10/1 to 8/1) to obtain 186 mg of the compound represented by formula (IIIc) in a yield of 44%.

At the same time, in my other blogs, there are other synthetic methods of this type of compound, 1-Bromo-2-isopropylbenzene, and friends who are interested can also refer to it.

Reference:
Patent; Tsinghua University; Wang Meixiang; Shi Tanhao; Guo Qinghui; Tong Shuo; (35 pag.)CN110372468; (2019); A;,
Bromide – Wikipedia,
bromide – Wiktionary