Month: June 2021

Some common heterocyclic compound, 4333-56-6, name is Bromocyclopropane, molecular formula is C3H5Br, 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. Recommanded Product: 4333-56-6

guanidine hydrochloride 100 kg with the bromo cyclopropane 126.6 kg placed in 800 kg in acetone, then adding the potassium carbonate 174.6 kg, heating to 50 C, reaction 3.5h, dropped to room temperature after-filtration, the filtrate is concentrated under reduced pressure to dry, to produce an intermediate 198.6 kg, molar yield 95%;

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 4333-56-6, its application will become more common.

Reference:
Patent; QILU SYNVA PHARMACEUTICAL CO., LTD.; LIU, ZHI; KONG, QINGWEN; FANG, MINGFENG; LIU, QUANCAI; KONG, MEI; WU, LIANYONG; (6 pag.)CN104649982; (2016); B;,
Bromide – Wikipedia,
bromide – Wiktionary

Synthetic Route of 1435-53-6, 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 1435-53-6 as follows.

General procedure: 8.3 1,3-Di(2′-methoxyphenyl)-4-fluorobenzene (11c): Starting with 10 (100 mg, 0.39 mmol), Cs2CO3 (253 mg, 0.78 mmol), Pd(PPh3)4 (3 mol%), 2-methoxyphenylboronic acid (94 mg, 78 mmol) and 1,4-dioxane (4 mL), 11c was isolated as a colorless solid (73 mg, 60%). Mp 99-100 C. 1H NMR (300 MHz, CDCl3): delta = 3.75, 3.75 (s, 3H, OCH3), 6.89-6.98 (m, 4H, ArH), 7.04-7.11 (m, 1H, ArH), 7.17-7.25 (m, 3H, ArH), 7.39-7.48 (m, 2H, ArH). 13C NMR (75 MHz, CDCl3): delta = 55.6, 55.7 (OCH3), 111.1 (CH), 111.2 (CH), 114.9 (d, J = 22.5 Hz, CH), 120.5 (CH), 120.9 (CH), 128.7 (2C), 125.7 (d, J = 15.8 Hz, C), 130.1 (d, J = 8.3 Hz, CH), 130.9 (2CH), 131.5 (2CH), 133.0 (d, J = 8.3 Hz, CH), 134.1 (d, J = 3.8 Hz, C), 157.1, 157.6 (C), 159.1 (d, J = 244.0 Hz, CF). 19F NMR (282 MHz, CDCl3): delta = -116.36 (CF). IR (ATR, cm-1): , 2959 (m), 2924 (m), 2852 (m), 2836 (m), 1577 (m), 1494 (s), 1455 (s), 1434 (m), 1390 (m), 1256 (m), 1228 (m), 1109 (m), 1022 (s), 825 (m), 792 (m), 825 (s), 792 (s), 748 (s), 625 (m), 597 (m), 544 (m). GC-MS (EI, 70 eV); m/z (%) = 308 (100) [M]+, 278 (13), 260 (6), 233 (10), 110 (3). HRMS (EI) calcd. for C20H17O2F[M]+: 308.12071; found 308.12018.

According to the analysis of related databases, 1435-53-6, the application of this compound in the production field has become more and more popular.

Reference:
Article; Sharif, Muhammad; Maalik, Aneela; Reimann, Sebastian; Feist, Holger; Iqbal, Jamshed; Patonay, Tamas; Villinger, Alexander; Langer, Peter; Journal of Fluorine Chemistry; vol. 146; (2013); p. 19 – 36;,
Bromide – Wikipedia,
bromide – Wiktionary

Application of 54962-75-3, These common heterocyclic compound, 54962-75-3, name is 3-Bromo-5-(trifluoromethyl)aniline, 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.

Preparation 30; [229] Preparation of 3-(4-methyl-imidazol- 1 – yl)-5-trifluoromethyl-phenylamine; [230] 3-amino-5-bromo-benzotrifluoride (17.1g,71.24mmol), 4-methylimidazole (17.6g,213.72mmol), potassium carbonate (9.8g, 71.24mmol), cupper (1. Ig, 17.81mmol), and cupper iode (II) (3.4g, 17.81mmol) were added to N,N-dimethylacetamide (100ml) at room temperature, and mixed therewith at 140~150C for 16 hr. After the reaction was completed, the temperature of the reaction vessel was cooled to RT. Then, ethyl acetate (200ml) was added thereto and mixed therewith for 30 min. The reaction mixture was filtered with Celite, and an organic layer of the filtered solution was washed with water, dried with magnesium sulfate, distilled under vacuum, and washed with n- hexane to give the titled compound as pale white solid.[231] 1H-NMR (CDCl3 delta)= 2.28 (s,3H), 4.04 (br,2H), 6.79 (s,lH), 6.83 (s,lH), 6.92(s,lH), 7.00 (s,lH), 7.77 (s.lH)

The synthetic route of 54962-75-3 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; IL-YANG PHARM. CO., LTD.; WO2007/18325; (2007); 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. 50548-45-3, name is 1-Bromodibenzo[b,d]furan, A new synthetic method of this compound is introduced below., category: bromides-buliding-blocks

20 g (80 mmol) of dibenzofuran-l-boronic acid, 2.06 g (40.1 mmol) of iodine, 3.13 g (17.8 mmol) of iodic acid, 80 ml of acetic acid, 5 ml of sulphuric acid, 5 ml of water and 2 ml of chloroform are stirred at 65 C. for 3 h. After cooling, the mixture is admixed with water, and the precipitated solids are filtered off with suction and washed three times with water. The residue is recrystallized from toluene and from dichloromethane/heptane. The yield is 25.6 g (68 mmol), corresponding to 85% of theory.

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; Merck Patent GmbH; PARHAM, Amir Hossain; EBERLE, Thomas; JATSCH, Anja; GROSSMANN, Tobias; KROEBER, Jonas Valentin; MONTENEGRO, Elvira; JOOSTEN, Dominik; WERN, Caroline; (238 pag.)US2019/119260; (2019); A1;,
Bromide – Wikipedia,
bromide – Wiktionary

Reference of 54962-75-3,Some common heterocyclic compound, 54962-75-3, name is 3-Bromo-5-(trifluoromethyl)aniline, molecular formula is C7H5BrF3N, 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.

3-Bromo-5-(trifluoromethyl)phenylamine (5 g, Alfa-Aesar) was dissolved in AcOH (140 ml) and Ac2O (5.9 ml, Aldrich) was added. The reaction was stirred at RT overnight. The mixture was added slowly to H2O (~700 ml) forming a white precipitate. The solid was isolated by filtration, washed with H2O and dried under vacuum to yield N-(3- , . bromo-5-1xifluoromethyl-phenyl)-acetamide.

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 3-Bromo-5-(trifluoromethyl)aniline, its application will become more common.

Reference:
Patent; AMGEN INC.; WO2007/48070; (2007); A2;,
Bromide – Wikipedia,
bromide – Wiktionary

Related Products of 90868-92-1, 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. 90868-92-1, name is (4-Bromophenyl)(cyclopropyl)methanamine belongs to bromides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

Production Example 29; To a mixture of 1-(4-bromophenyl)-1-cyclopropylmethane amine (1.08 g) and THF (10 mL) were added triethylamine (1 mL) and di-tert-butyl dicarbonate (1.25 mL), and the mixture was stirred at room temperature for 16 hours. The solvent was concentrated under reduced pressure, and the obtained residue was purified by silica gel column chromatography (hexane-ethyl acetate) to obtain tert-butyl [(4-bromophenyl)(cyclopropyl)methyl]carbamate (1.36 g).

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-Bromophenyl)(cyclopropyl)methanamine, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; Astellas Pharma Inc.; EP2277858; (2011); A1;,
Bromide – Wikipedia,
bromide – Wiktionary

630-17-1, name is 1-Bromo-2,2-dimethylpropane, 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. Recommanded Product: 1-Bromo-2,2-dimethylpropane

l-(2,2-dimethylpropyI)-4-fluoro-S-methoxy-3-met yl-l,3-dihydro-2H-benzimidazol~2-one (7-5)A solution of 7-fluoro-6-methoxy-l -methyl- 1 ,3 -dihydro-2H-benzimidazol-2-one (7-4, 250 mg, 1.27 mmol) in anhydrous DMF (1.5 ml) was treated with NaH and l-Bromo-2,2- dimethylpropane. The reaction was then irradiated in a microwave at 175 deg C for 25 min. The reaction was partitioned between EtOAc (2×60 ml) and water (75 ml). The combined organic layers were dried over Na2S04 and concentrated, affording the title compound, 1 -(2,2- dimethylpropyl)-4-fluoro-5-methoxy-3-methyl-l,3-dihydro-2H-benzimidazol-2-one (7-5), as an orange oil. 1HNMR (300 MHz, CDC13) delta 6.65-6.70 (m, 2H), 3.88 (s, 3H), 3.60 (m, 5H)} 1.03 (s, 9H). LRMS m/z Calc’d for Ci4Hi9FN202 (M+H) 267.3, found 267.0.

The synthetic route of 630-17-1 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; MERCK SHARP & DOHME CORP.; DUDKIN, Vadim; FRALEY, Mark, E.; ARRINGTON, Kenneth, L.; LAYTON, Mark, E.; RODZINAK, Kevin, J.; PERO, Joseph, E.; REIF, Alexander, J.; WO2012/21382; (2012); A1;,
Bromide – Wikipedia,
bromide – Wiktionary

Adding a certain compound to certain chemical reactions, such as: 89523-51-3, name is 5-Bromobenzo[c]phenanthrene, 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 89523-51-3, Application In Synthesis of 5-Bromobenzo[c]phenanthrene

Under an argon atmosphere, 10.1g g of 5-bromobenzo[c] phenanthrene which had been prepared in Synthesis Example 1 was placed in a flask. 400 mL of dehydrated ether was added to this flask. The reaction solution was cooled to -40 C, and 22 ml of 1.6M hexane solution of n-butyllithium was added. The resultant was heated to 0 C, and stirred for an hour. The reaction solution was cooled to -60 C, and 10 mL. of a dehydrated ether solution of 14.4g of triisopropyl borate was dripped. The reaction solution was stirred for 5 hours while heating to room temperature. 100 mL of a 10% hydrochloric acid solution was added and the mixture was stirred for an hour. An aqueous phase was removed, and an organic phase which had been separated was washed with water and saturated brine, and then dried with magnesium sulfate. After the magnesium sulfate was filtered out, the organic phase was concentrated. The solids obtained were washed with hexane, whereby 5.37g (yield: 60%) of benzo[c]phenanthrene-5-boronic acid was obtained.

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, 5-Bromobenzo[c]phenanthrene, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; Idemitsu Kosan Co., Ltd.; EP2218706; (2010); A1;,
Bromide – Wikipedia,
bromide – Wiktionary

Some common heterocyclic compound, 1073-06-9, name is 1-Bromo-3-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. Application In Synthesis of 1-Bromo-3-fluorobenzene

A nitrogen-protected four-necked flask was charged with 268 g of diisopropylamine and 100 g of tetrahydrofuran, cooled to -40 C to -50 C, and 340 g was added dropwise at -40 C to -50 C Butyl lithium, stirring and holding 1 hour, the raw material reaction is completed. Cooling to -70 ~ -80 ,A mixture of 200 g of fluorobromobenzene and 100 g of tetrahydrofuran was added dropwise,Stir for 2 hours. After the addition of dimethylformamide 112 g, stirring for 1 hour, hydrochloric acid quenching pH = 1 ~ 2.The ethyl acetate extract was distilled under vacuum under reduced pressure to give 165 g of 2-fluoro-6-bromobenzaldehyde and 98% pure GC.

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 1073-06-9, its application will become more common.

Reference:
Patent; Dalian Lianhua Chemical Co., Ltd.; Liu Qibin; Wang Zhongxing; (5 pag.)CN106977535; (2017); A;,
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. 3972-64-3, name is 1-Bromo-3-(tert-butyl)benzene belongs to bromides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below. Formula: C10H13Br

[0252] A mixture of intermediate 32 (298 mg, 1.0 mmol), 1 -tert-butyl-3 -bromobenzene (256 mg, 1.2 mmol), Pd2(dba)3 (92 mg, 0.1 mmol), Xantphos (180 mg, 0.3 mmol) and cesium carbonate (1.3 g, 4 mmol) was suspended in dioxane (50 mL) and heated at reflux under the argon atmosphere for 20 h. The mixture was filtered and the filtrate concentrated in vacuo. The residue was purified by HPLC to afford the title compound (27 mg of HCl salt, 6percent) as a white solid.[0253] 1H NMR (500 MHz, DMSOd6): delta 1.25 (s, 9H), 2.16 (s, 3H), 2.80 (d, J= 4.6 Hz, 3H), 3.04-3.16 (m, 4H), 3.47-3.49 (m, 2H), 3.65-3.67 (m, 2H), 6.90 (d, J= 8.9 Hz, 2H), 7.26 (d, J = 9.0 Hz, 2H), 7.28-7.35 (m, 2H), 7.45 (t, J= 1.8 Hz, IH), 7.50 (d, J= 7.8 Hz, IH), 7.86 (s, IH), 9.70 (s, IH), 10.37 (s, IH), 11.01 (br s, IH), 12.34 (br s, H). MS (ES+): m/z 431 . (M+H)+.

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

Reference:
Patent; TARGEGEN, INC.; WO2007/53452; (2007); A1;,
Bromide – Wikipedia,
bromide – Wiktionary