Month: May 2021

Application of 707-34-6, 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. 707-34-6 name is 1,3,5-Tribromoadamantane, 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.

Step seven, equipped with a condenser, a thermometer four 5L reaction flask were successively added 473g1.3.5- tribromo adamantane, 946 g silver sulfate, 946 g of water and 94.6ml of toluene, stirring was started, 946 g of concentrated sulfuric acid was added dropwise, complete after the temperature was raised to about 110 deg.] C under reflux for 16 hours. (2 in the control) document.write(“”); Step 8 After completion of the reaction, the temperature was lowered to room temperature, filtered, the filter cake was washed with 700ml of water and the combined filtrate, the filtrate was added 250g sodium bromide was stirred for half an hour excess silver ions precipitate was filtered, the filter cake was washed with 300ml of water, combined filtrate. The filtrate was diluted with 500ml of water was added.document.write(“”); Step 9 using 30% sodium hydroxide solution PH = 12-13, at a temperature controlled above 75 , use up to about 2850 g of liquid caustic soda, After completion, it was cooled to 25-30 & deg.] C slowly, stirred for 30min, filtered, and collected by filtration cake. document.write(“”); Step 10, the filter cake was added to 1.8L of methanol, 57g of activated carbon, stirred for IH, filtered, and the filtrate was recovered white paste, into 1.5L petroleum ether was filtered to give the product as a white solid 210g. (3 in the control)

At the same time, in my other blogs, there are other synthetic methods of this type of compound, 1,3,5-Tribromoadamantane, and friends who are interested can also refer to it.

Reference:
Patent; XuzhouBokang Information Chemicals co., LTD; FU, ZHIWEI; (9 pag.)CN104628526; (2016); B;,
Bromide – Wikipedia,
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Adding a certain compound to certain chemical reactions, such as: 768-90-1, name is 1-Bromoadamantane, 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 768-90-1, Computed Properties of C10H15Br

General procedure: Benzo[b]thiophene-3-carbaldehyde (40 mg, 0.25 mmol, 1.0 equiv),Pd(TFA) 2 (4.2 mg, 5 mol%), (4-FC 6 H 4 ) 3 P (9.5 mg, 12 mol%), DPEphos (8mg, 6 mol%), and Cs 2 CO 3 (122 mg, 0.375 mmol) were placed in atransparent Schlenk tube equipped with a stirring bar. The tube wasevacuated and filled with argon for three times. Degassed DMF (2.5mL) and tert-butyl bromide (51 mg, 0.375 mmol, 1.5 equiv) were add-ed via a gastight syringe. The reaction mixture was stirred under theirradiation of 36 W blue LEDs (distance app. 2.0-3.0 cm from thebulb) at r.t. for 24 h. The mixture was quenched with brine and ex-tracted with EtOAc (3 × 10 mL). The organic layers were combinedand concentrated under reduced pressure. The product was purifiedby flash column chromatography on silica gel using PE or a mixture of PEand EtOAc (10:1 v/v) as eluent; yield: 50.1 mg (92%); pale yellow liquid.

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:
Article; Wang, Guang-Zu; Shang, Rui; Fu, Yao; Synthesis; vol. 50; 15; (2018); p. 2908 – 2914;,
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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. 21865-50-9, name is 6-Bromo-2,3,4,9-tetrahydro-1H-carbazole, This compound has unique chemical properties. The synthetic route is as follows., name: 6-Bromo-2,3,4,9-tetrahydro-1H-carbazole

23.6 g (63.17 mmol) of the compound represented by the formula [1-b] obtained from the above-mentioned scheme 2 and 3.3 g (82.1 mmol) of 60% sodium hydride were placed in 200 ml of dimethylformamide and stirred at room temperature for 30 minutes . Thereafter, 15.7 g (63.17 mmol) of the compound represented by the formula [3-b] obtained from the above-mentioned Reaction Scheme 13 was dissolved in 150 ml of dimethylformamide, and the mixture was slowly added dropwise, followed by stirring for 1 hour. After completion of the reaction, 20 ml of distilled water was added, followed by filtration and recrystallization to obtain 16.0 g of a compound represented by the formula (3-c). (Yield: 43%)

According to the analysis of related databases, 21865-50-9, the application of this compound in the production field has become more and more popular.

Reference:
Patent; SFC Ltd.; P’yo Seong-wan; Lee Se-jin; (61 pag.)KR101970987; (2019); B1;,
Bromide – Wikipedia,
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Adding a certain compound to certain chemical reactions, such as: 6698-13-1, name is 4-Bromo-1,3-benzodioxole, 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 6698-13-1, COA of Formula: C7H5BrO2

Step A: 4-Benzo[1,3]dioxol-4-yl-3,6-dihydro-2H-pyridine-1-carboxylic acid tert-butyl esterTert-butyl 4-(4,4,5,5-tetramethyl-1,3,2-dioxaborolan-2-yl)-5,6-dihydropyridine-1(2H)-carboxylate (1.62 g, 5.22 mmol) was added to a solution of 4-bromobenzo[d][1,3]dioxole (1 g, 4.97 mmol) in 1,2-Dimethoxyethane (45.0 ml) and Na2CO3 2M (8.28 ml, 16.6 mmol). The resulting suspension was degassed using a stream of argon in an ultrasonic bath during 5 min. Then triphenylphosphine (261 mg, 995 mumol) and palladium (II) acetate (112 mg, 497 mumol) was added and the reaction mixture was stirred over night at 85 C. The reaction was cooled to rt, diluted with 40 mL of water and the mixture extracted with ethyl acetate (3×50 mL). The organic layers were dried over MgSO4 and concentrated under vacuum. The crude material was purified by flash chromatography (silica gel, 50 g, 0% to 50% EtOAc in heptane) to yield 4-Benzo[1,3]dioxol-4-yl-3,6-dihydro-2H-pyridine-1-carboxylic acid tert-butyl ester as a yellowish liquid (1.22 g, 80.8%). MS (ISP) m/z=304.4 [(M+H)+].

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; Rodriguez Sarmiento, Rosa Maria; Wichmann, Juergen; US2012/225868; (2012); A1;,
Bromide – Wikipedia,
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Synthetic Route of 90562-10-0, 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. 90562-10-0, name is 1-Bromo-4-(3-bromopropyl)benzene belongs to bromides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

(41-4) Synthesis of [5-(2-{4-[3-(4-bromophenyl)propoxy]-3-trifluoromethylphenyl}ethyl)-2,2-dimethyl-1,3-dioxan-5-yl]carbamic acid t-butyl ester (compound 41-4) Reference Example compound 2-6 (500 mg) was dissolved in N,N-dimethylformamide (10 ml), potassium carbonate (494 mg) and compound 41-3 (447 mg) were added, and the mixture was stirred at 80C for 1.5 hr. Water was added to the reaction mixture, and the mixture was extracted with ethyl acetate, washed with water and saturated brine, and dried over anhydrous magnesium sulfate. The solvent was evaporated under reduced pressure to give the object product (820 mg) as a white solid. 1H-NMR(CDCl3) 5 (ppm): 1.43(3H, s), 1.44(3H, s), 1.47(9H, s), 1.93-1.98(2H, m), 2.06-2.10(2H, m), 2.51-2.56(2H, m), 2.77-2.81(2H, m), 3.69(2H, d, J=11.7Hz), 3.89(2H, d, J=11.7Hz), 3.96(2H, t, J=6.0Hz), 5.00(1H, brs), 6.83(1H, d, J=8.5Hz), 7.05-7.09(2H, m), 7.24-7.27(1H, m), 7.36-7.43(3H, m).

The synthetic route of 1-Bromo-4-(3-bromopropyl)benzene has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Mitsubishi Tanabe Pharma Corporation; EP2168944; (2010); A1;,
Bromide – Wikipedia,
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These common heterocyclic compound, 35354-37-1, name is 1-Bromo-5-methylhexane, 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

Example 145 (+-)-4-(3-Ethanesulfonylaminophenyl)-trans-3,4-dimethyl-N-(5-methylhexyl)piperidine To a stirred solution of (+-)4-(3-ethanesulfonylaminophenyl)-trans-3,4-dimethylpiperidine (Preparation 39, 120 mg, 0.4 mmol) in N,N-dimethylformamide (7 ml) was added sodium hydrogen carbonate (68 mg, 0.8 mmol) and 1-bromo-5-methylhexane (80 mg, 0.44 mmol). The stirred reaction mixture was heated to 100° C. for 16 h, then allowed to cool. Water (50 ml) was added and the mixture was extracted with diethyl ether (3*50 ml). The combined extracts were washed with brine (50 ml), dried (Na2SO4), filtered and concentrated in vacuo. The residue was purified by silica (5 g) column chromatography eluding initially with hexane, then hexane:ethyl acetate:0.880 ammonia (50:50:1) to give a yellow oil (15 mg). The residue was further purified by preparative HPLC on a Phenomenex Magellan.(TM). column, 15 cm*2.1 cm; flow 10.0 ml min-1; employing U.V. detection at 235 nm; eluant acetonitrile:0.1M aqueous ammonium acetate solution:methanol (25:35:40) to afford the title compound as its acetate salt as a yellow oil (10 mg, 6percent). NMR (CDCl3, selected data for the acetate salt): 0.8 (d, 3H), 1.8 (m, 1H), 2.4 (m, 1H), 2.85 (m, 1H), 3.1 (q, 2H), 7.05-7.3 (m, 4H). MS (APCI): M/Z [MH+] 395.2; C22H38N2O2S+H requires 395.3.

The synthetic route of 1-Bromo-5-methylhexane has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Armer, Richard Edward; Dutton, Christopher James; Gethin, David Morris; Gibson, Stephen Paul; Smith, Julian Duncan; Tommasini, Ivan; US2003/78282; (2003); A1;,
Bromide – Wikipedia,
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Adding a certain compound to certain chemical reactions, such as: 106-37-6, name is 1,4-Dibromobenzene, 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 106-37-6, Recommanded Product: 106-37-6

1 Synthesis of 4-Decylbromobenzene: In a reaction flask were charged 10.2 g of metallic magnesium, 100 ml of THF, and a small amount of iodine in a nitrogen stream, and a part of 500 ml of a THF solution containing 100 g of 1,4-dibromobenzene was added thereto dropwise to initiate reaction. Then, the rest of the solution was added dropwise at 25 to 30 C. over a 2-hour period, and the mixture was allowed to react at 40 C. for 1 hour, followed by cooling to prepare a Grignard reagent. Separately, 187 g of decyl bromide, 500 ml of benzene, 98.3 g of N,N,N’,N’-tetramethylethylenediamine, and 2.1 g of copper (I) chloride were put in a reaction flask, and the atmosphere was displaced with nitrogen. The mixture was heated to 50 C., and the above prepared Grignard reagent was added thereto dropwise at that temperature over 30 minutes. The reaction mixture was allowed to react for 24 hours, cooled, and poured into a saturated aqueous ammonium solution, and extracted with ethyl acetate. The extract was washed with water and dried over magnesium sulfate to recover 107 g of a crude product. The crude product was distilled in a Claisen flask equipped with a Vigreaux tube cylinder to obtain 43.7 g of the title compound.

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

Reference:
Patent; Takasago International Corporation; US5716542; (1998); A;,
Bromide – Wikipedia,
bromide – Wiktionary

Electric Literature of 1435-54-7,Some common heterocyclic compound, 1435-54-7, name is 1,3-Dibromo-2-fluorobenzene, molecular formula is C6H3Br2F, 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-isopropylphenol 0.1mol, dissolved in 100mL anhydrous tetrahydrofuran, stirring, accurately weighed 0.4mol sodium hydride in batches added to the reaction bottle, not too fast to prevent too much bubbles. After adding the solution turned yellow, then add 1,3-dibromo-2-fluorobenzene 0.11mol, also added in batches, room temperature overnight. The resulting reaction product was filtered to remove the solid material, the filtrate was dry and dissolved in dichloromethane. The column was washed with petroleum ether: ethyl acetate = 1: 5 (volume ratio) to give 1,3-dibromo-2-(2-isopropylphenoxy)benzene (Intermediate A-1) (0.05 mol, y = 50%).

The synthetic route of 1435-54-7 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Jilin Optical and Electronic Materials Co., Ltd.; Cui, Dunzhu; Gao, Chunji; Wang, Hui; Ma, Xiaoyu; Zhao, He; Li, Ming; Li, Wenjun; (65 pag.)CN106146538; (2016); A;,
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Application of 959992-62-2, These common heterocyclic compound, 959992-62-2, name is 6-Bromo-3,4-dihydro-2H-pyrido[3,2-b][1,4]oxazine, 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.

Example 1173-((3,4-Dihydro-2H-pyrido[3,2-b][1,4]oxazin-6-yl)ethynyl)-7,7-dimethyl-7,8- dihydroquinolin-5(6H)-one[00323]The synthesis of 6-bromo-3,4-dihydro-2/-/-pyrido[3,2-b][1 ,4]oxazine is described in literature (e.g., WO 2007/141473).[00324]A mixture of 6-bromo-3,4-dihydro-2/-/-pyrido[3,2-b][1 ,4]oxazine (107 mg, 0.50 mmol), PdCI2[PPh3]2 (35 mg, 0.05 mmol), and Cul (10 mg, 0.05 mmol) in anhydrous acetonitrile (5 mL) is degassed. Then 3-ethynyl-7,7-dimethyl-7,8-dihydroquinolin-5(6/-/)- one (100 mg, 0.50 mmol) is added followed by TEA (1 mL). The reaction mixture is stirred under argon atmosphere at 60 C for 8 h, cooled down to r.t. and concentrated at reduced pressure. The obtained residue is purified by preparative HPLC (C18, acetonitrile/water) to provide the title compound (32 mg, 20%).1H NMR (CDCI3), deltaEta, 1 .12 (s, 6H), 2.56 (s, 2H), 3.05 (s, 2H), 3.58 (t, 2H), 4.26 (t, 2H), 5.07 (br s, 1 H), 6.89 (d, 1 H), 6.96 (d, 1 H), 8.38 (s, 1 H), 8.84 (s, 1 H).LC/MS (M+H)+ = 334, 375

The synthetic route of 959992-62-2 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; MERZ PHARMA GMBH & CO. KGAA; HENRICH, Markus; ABEL, Ulrich; MULLER, Sibylle; KUBAS, Holger; MEYER, Udo; HECHENBERGER, Mirko; KAUSS, Valerjans; ZEMRIBO, Ronalds; WO2012/52451; (2012); A1;,
Bromide – Wikipedia,
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Reference of 6698-13-1,Some common heterocyclic compound, 6698-13-1, name is 4-Bromo-1,3-benzodioxole, molecular formula is C7H5BrO2, 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.

4.1.3.1. 1-(Benzofuran-7-yl)-3-(dimethylamino)propan-1-one (V:class D-7). A solution of 7-bromobenzofuran (2.05 g, 10.4 mmol)in dry THF (20 mL) was prepared. Approximately 4 mL of this solutionwas added to a flask containing magnesium (0.75 g, 30.9mmol) and the mixture was agitated until an exothermic reactionoccurred. The remaining solution was added and the mixture wasrefluxed for 1 h, cooled and transferred by cannula to a dry flask.The solution was cooled to 0 C and acetaldehyde (0.70 mL, 12.3mmol) was added, the mixture was stirred at 0 C for 1 h then partitionedbetween EtOAc and water, the organic fractions were dried and evaporated. Column chromatography with hexanes:DCM(1:1) eluted non polar impurities, elution with DCM

The synthetic route of 6698-13-1 has been constantly updated, and we look forward to future research findings.

Reference:
Article; Sutherland, Hamish S.; Tong, Amy S.T.; Choi, Peter J.; Conole, Daniel; Blaser, Adrian; Franzblau, Scott G.; Cooper, Christopher B.; Upton, Anna M.; Lotlikar, Manisha U.; Denny, William A.; Palmer, Brian D.; Bioorganic and Medicinal Chemistry; vol. 26; 8; (2018); p. 1797 – 1809;,
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