Author: tianli

Related Products of 630-17-1, These common heterocyclic compound, 630-17-1, name is 1-Bromo-2,2-dimethylpropane, 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.

General procedure: A 10 mL Schlenk tube was charged with CoBr2 (6.6 mg, 0.03mmol), 1,3-diisopropyl-1H-benzimidazol-3-ium bromide (L4; 8.5mg, 0.03 mmol), 4-methoxy-N-[(1E)-1-phenylethylidene]aniline(1a, 67.6 mg, 0.30 mmol), 1-chlorooctane (2a, 76.5 muL, 0.45 mmol), and THF (0.69 mL). A 1.92 M solution of t-BuCH2MgBr inTHF (0.31 mL, 0.60 mmol) was added dropwise at 0 C, and themixture was stirred at r.t. for 6 h. The reaction was quenched by theaddition of 3 M aq HCl (1.0 mL), and the mixture was stirred at r.t.for 1 h, then extracted with EtOAc (3 ¡Á 10 mL). The organic layerswere combined, dried (MgSO4), and concentrated under reduced pressure. The crude product was purified by chromatography [silicagel, hexane-EtOAc (40:1)].

Statistics shows that 1-Bromo-2,2-dimethylpropane is playing an increasingly important role. we look forward to future research findings about 630-17-1.

Reference:
Article; Gao, Ke; Yamakawa, Takeshi; Yoshikai, Naohiko; Synthesis; vol. 46; 15; (2014); p. 2024 – 2039;,
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. 52997-43-0, name is 7-(Bromomethyl)pentadecane, A new synthetic method of this compound is introduced below., SDS of cas: 52997-43-0

General procedure: General procedure for the synthesis of a1-a6: To a solution of indoline-2,3-diones (10 mmol) in DMF (40 mL) was added K2CO3(15 mmol, 2.073 g) and 7-(bromomethyl)pentadecane (11 mmol,3.358 g) under nitrogen. The mixture was stirred at 70 C and monitoredby TLC. After the reaction completed, water was added, andextracted with EtOAc. The organic layer was combined and dried withMgSO4. After evaporation of the solvent, the residue was purified bycolumn chromatograph (eluent: Petroleum/EtOAc=20:1) to give thetarget compound.

The synthetic route of 52997-43-0 has been constantly updated, and we look forward to future research findings.

Reference:
Article; Hu, Qian; Jiang, Hua; Cui, Zhihua; Chen, Weiguo; Dyes and Pigments; vol. 173; (2020);,
Bromide – Wikipedia,
bromide – Wiktionary

Synthetic Route of 112279-72-8, 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. 112279-72-8 name is 4-Bromo-2,3-difluoroaniline, 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.

N-((4-bromo-2,3-difluorophenyl)carbamothioyl)benzamide was prepared according to the following procedure. To 4-bromo-2,3-difluoroaniline (3.70 g, 17.8 mmol) dissolved in acetone (20 mL) was added benzoyl isothiocyanate (2.90 g, 2.39 mL, 1 eq, 17.8 mmol) drop-wise. The reaction was stirred for 30 min at 18 C, the mixture was filtered, the collected white solid was washed with heptane (50 mL) and vacuum dried to afford N-((4-bromo-2,3-difluorophenyl)carbamothioyl)benzamide (5.68 g, 85%) as a white solid.?H NMR (300 MHz, DMSO-ifc) d 12.45 (s, 1H), 11.91 (s, 1H), 8.46 – 7.88 (m, 2H), 7.78 – 7.26 (m, 6H).

At the same time, in my other blogs, there are other synthetic methods of this type of compound, 4-Bromo-2,3-difluoroaniline, and friends who are interested can also refer to it.

Reference:
Patent; ACUCELA INC.; ORME, Mark, W.; ZUNIGA, Edison, S.; KUKSA, Vladimir, A.; CRAFT, Russell, Stuart; SAVEEDRA, Eduardo, Moreno; MEISSNER, Johannes, Wilhelm, Georg; DEN HARTOG, Jacobus, Antonius, Joseph; DROS, Albert, Cornelis; (223 pag.)WO2020/69330; (2020); 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. 43204-63-3, name is Bis(2-Bromoethyl)amine hydrobromide, A new synthetic method of this compound is introduced below., HPLC of Formula: C4H10Br3N

Step 4: 4,5-Difluoro-2-(piperazin-1-yl)benzenesulfonamide A mixture of 2-amino-4,5-difluoro-benzenesulfonamide (1.04 g, 5.00 mmol), 2-bromo-N-(2-bromoethyl)ethanamine hydrobromide (15.59 g, 50.00 mmol) and n-butyl alcohol (50.00 mL) was stirred at 120 C. for 40 h. The reaction mixture was filtered and the filtrate was concentrated in vacuo. The residue was purified via preparative HPLC to afford 4,5-difluoro-2-piperazin-1-yl-benzenesulfonamide (400.00 mg, 1.15 mmol, 23% yield, 80% purity) as a white solid. MS (EI+, m/z): 278.1 [M+H]+.

The synthetic route of 43204-63-3 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Navitor Pharmaceuticals, Inc.; O’Neill, David John; Saiah, Eddine; Kang, Seong Woo Anthony; Brearley, Andrew; Bentley, Jonathan; (519 pag.)US2018/127370; (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. 18648-66-3, name is 2-(4-Bromophenyl)-1,1-diphenylethylene, A new synthetic method of this compound is introduced below., HPLC of Formula: C20H15Br

P-aminobenzeneboronic acid hydrochloride was added1000ml three-necked flask, add 800ml tetrahydrofuran, then add 2mol / L potassium carbonate solution 168ml, magnetic stirring and argon, oil bath heated to 70 , adding 0.1g tetraphenylphenylphosphine palladium, reflux reaction 24h, The reaction product was spin-dried and the product was spin-dried to dry the powder and dried in vacuo at 60 C for 24 h to give the white intermediate TriP-NH2 in 86% yield.

The synthetic route of 18648-66-3 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Sun Yat-sen University; Zhang, Yi; Liu, Yiwu; Xu, Jiarui; Wu, Xinhui; Shi, Jie; Liu, Siwei; Chi, Zhenguo; (20 pag.)CN104341311; (2016); B;,
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. 74586-53-1, name is 3-Bromo-5-methylaniline, This compound has unique chemical properties. The synthetic route is as follows., Product Details of 74586-53-1

Preparative Example 1.2 – N-(3-b yclopropylpyrimidin-2-amine To a solution of 2-chloro-4-cyclopropyl-pyrimidine (12.5 g, 81 mmol) and 3- bromo-5-methylaniline (18.1 g, 97 mmol) in 1,4-dioxane (100 mL) was added pivalic acid (9.3 mL, 81 mmol). The resulting mixture was heated to reflux and left stirring for 10 hours. The mixture was allowed to cool to room temperature and hexanes were added (80 mL). The slurry was filtered and the filtrate was washed with MeOH to afford a portion of N-(3-bromo-5- methylphenyl)-4-cyclopropylpyrimidin-2-amine. The mother liquors were concentrated, absorbed on silica gel and purified by silica gel column chromatography (EtO Ac/Hex) to afford additional N-(3-bromo-5-methylphenyl)-4-cyclopropylpyrimidin-2-amine as a white solid. MS ESI calcd. for C14H15BrN3 [M+H]+ 304 and 306, found 304 and 306.

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 74586-53-1.

Reference:
Patent; MERCK SHARP & DOHME CORP.; MERCK CANADA INC.; HAIDLE, Andrew, M.; BURCH, Jason; GUAY, Daniel; GAUTHIER, Jacques Yves; ROBICHAUD, Joel; FOURNIER, Jean Francois; ELLIS, John Michael; CHRISTOPHER, Matthew; KATTAR, Solomon, D.; SMITH, Graham; NORTHRUP, Alan, B.; WO2014/31438; (2014); A2;,
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. 7499-66-3, name is 6-Bromonaphthalen-2-amine belongs to bromides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below. Recommanded Product: 6-Bromonaphthalen-2-amine

Example 15 Synthesis of 2-bromo-6-(N-methylamino)Naphthalene (Intermediate 27) A solution of 2-amino-6-bromonaphthalene (2.0 g) in 1,4-dioxane (30 ml) was added dropwise with dimethyl sulfate (1300 mul) and stirred at room temperature for 46 hours.The reaction mixture was added with ethyl acetate (90 ml) and then added with 1 N aqueous sodium hydroxide (5 ml).This mixture was extracted with ethyl acetate (150 ml*3).The organic layer was washed with saturated brine and dried, and then the solvent was evaporated under reduced pressure.The residue was purified by flash column chromatography (hexane:ethyl acetate=15:1) to obtain the title compound (Intermediate 27, 152 mg).

The synthetic route of 7499-66-3 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Shoda, Motoshi; Kuriyama, Hiroshi; US2004/44258; (2004); A1;,
Bromide – Wikipedia,
bromide – Wiktionary

Related Products of 937046-98-5, 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. 937046-98-5, name is 7-Bromopyrrolo[2,1-f][1,2,4]triazin-4-amine belongs to bromides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

A 3-L round bottom flask equipped with a mechanical stirrer, a heating mantle, a thermal couple, a reflux condenser, a nitrogen inlet and a nitrogen outlet was charged with 7- bromopyrrolo[2,1-f][1,2,4]triazin-4-amine (Compound 11, 100 g, 469 mmol) and tert- butyl 4-(4,4,5,5-tetramethyl- 1,3,2-dioxaborolan-2-yl)-5,6-dihydropyridine- 1 (2T/)-carboxylate (Compound 12, 174 g, 563 mmol) in l,4-dioxane (876 mL) at room temperature. To the reaction flask was added potassium carbonate (130 g, 939 mmol) and water (218 g) in sequence. The mixture was degassed by exposure to vacuum and refilled with nitrogen atmosphere for three times. After the addition of tetrakis(triphenylphosphine)palladium (0) (Pd(PPh3)4, 13.56 g, 11.7 mmol), the reaction mixture was degassed and refilled with nitrogen for three times at room temperature. Then the reaction mixture was heated to 85 – 90 C, and agitated at that temperature for 16 hours. Upon the completion of the reaction, water (900 mL) was added in 30 minutes while the internal temperature was above 50 C. The mixture was cooled to room temperature. Solids gradually precipitated out. The solids were collected by filtration at 18 C, and washed with water (2 x 250 mL) and methyl /eN-butyl ether (MTBE, 3 x 200 mL). The wet cake was put back into the reaction flask, and agitated in MTBE (750 mL) at 50 C for 1 hour. The solids were collected at room temperature by filtration. The cake was dried in a vacuum oven at 50 C under vacuum with nitrogen sweeping for 72 hours to provide tert-butyl 4-(4-aminopyrrolo[2,1-f][1,2,4]triazin-7-yl)-5,6- dihydropyridine- 1 (2H)-carboxylate (Compound 13, 123.7 g, 84%) as a brown solid. ‘H NMR (500 MHz, DMSO-i) d 7.89 (s, 1H), 7.69 (s, 2H), 7.00 (s, 1H), 6.91 (d, J= 4.6 Hz, 1H), 6.69 (d, J= 4.5 Hz, 1H), 4.06 (s, 2H), 3.55 (t, J= 5.5 Hz, 2H), 2.59 – 2.52 (m, 2H), 1.43 (s, 9H) ppm; C16H21N5O2 (MW 315.37), LCMS (El) m/e 316.1 (M+ + H).

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, 7-Bromopyrrolo[2,1-f][1,2,4]triazin-4-amine, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; INCYTE CORPORATION; ROCCO, William L.; MULLER, Francis X.; (0 pag.)WO2020/6408; (2020); A1;,
Bromide – Wikipedia,
bromide – Wiktionary

33070-32-5, name is 5-Bromo-2,2-difluorobenzodioxole, 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. name: 5-Bromo-2,2-difluorobenzodioxole

Example 1 : 3-(2,2-Difluoro-benzo[1 ,31dioxol-5-ylmethyl)-piperidine-1 -carboxylic acid pyridin-3-ylannide.Step A: 3-(2,2-Difluoro-benzo[1.SIdioxol-delta-ylnnethvD-piperidine-i-carboxylic acid tert-butyl ester.; 1 -Boc-3-methylene piperidine (842 mg, 4.27 mmol) was degassed (neat) for 15 minutes and then treated with a THF solution of 9-BBN (0.5 M in THF, 8.6 ml_, 4.3 mmol). The reaction mixture was refluxed for 2 h, then cooled to rt. The reaction mixture was then added, via cannula, to a preformed solution of 5-bromo-2,2-difluoro-1 ,3-benzodioxole (1.00 g, 4.22 mmol), Pd(dppf)CI2?CH2CI2 (94 mg, 0.128 mmol), and potassium carbonate (746 mg, 5.40 mmol) in DMF/H2O (10 mL/1 ml_). The resultant mixture was heated at 60 0C for 18 h, cooled to rt, poured into water, basified to pH 11 with 1 N NaOH, and extracted with EtOAc (3x). The organic layers were combined, dried (Na2SO4), and concentrated. The crude residue was purified (FCC) to give 3-(2,2-difluoro-benzo[1 ,3]dioxol-5-ylmethyl)- piperidine-1 -carboxylic acid tert-butyl ester (1.00 g, 67%).

The synthetic route of 33070-32-5 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; JANSSEN PHARMACEUTICA NV; BREITENBUCHER, J., Guy; KEITH, John, M.; TICHENOR, Mark, S.; CHAMBERS, Alison, L.; JONES, William, M.; HAWRYLUK, Natalie, A.; TIMMONS, Amy, K.; MERIT, Jeffrey, E.; SEIERSTAD, Mark, J.; WO2010/68452; (2010); A1;,
Bromide – Wikipedia,
bromide – Wiktionary

Adding a certain compound to certain chemical reactions, such as: 2924-09-6, name is 5-Bromo-2-fluoroaniline, 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 2924-09-6, SDS of cas: 2924-09-6

A solution of 5-bromo-2-fluoroaniline (10 g, 52 mmol) in toluene (150 ml) was treated with 4-bromobutyryl chloride (6.1 ml, 52 mmol) and then heated at [100C] for 14 h. The reaction was cooled then washed with water, 10% sodium carbonate, IN HCl and water, dried over anhydrous magnesium sulphate, filtered and concentrated im vacuo. The resulting tan solid was triturated with 5% ether in isohexane and collected by filtration to afford [4-BROMO-N- (5-BROMO-2-FLUOROPHENYL)] butyramide. This solid was dissolved in anhydrous [NN-DIMETHYLFORMAMIDE] (150 ml) then treated with sodium hydride (1.4 g of a 60% dispersion in oil) added in portions over 5 min. The resulting mixture was stirred at [60C] for 60 min, cooled and treated with methanol (10 ml). The reaction was diluted with water (1500 ml) and extracted with ether (2 x 400 ml). The organics were combined, washed with water (x 3), brine, dried over anhydrous magnesium sulphate, filtered and pre-adsorbed onto silica. Chromatography on silica gel, eluting with isohexane on a gradient of ethyl acetate (20-50%), gave [1- (5-BROMO-2-FLUOROPHENYL)] pyrrolidin-2-one (9.1 g, [67%)] as a straw-coloured solid: [8H] (400 MHz, CDCl3) 2.17-2. 25 (2H, m), 2. [55-2.] 59 (2H, m), 3. [80-3.] 84 (2H, m), 7.20 [(1H,] dd, J 10.5 and 9), 7.33- 7.37 [(1H,] m), 7.59 [(1H,] dd, J 7 and 2.5). 2-(8-Fluoroimidazo[1,2-a]pyridin-7-yl) propan-2-ol was coupled to [1-] (5-bromo-2-fluorophenyl) pyrrolidin-2-one as described in Example 6 to give [L- {2-NUORO-5- [8-FLUORO-7- (L-HYDROXY-L-METHYLETHYL)] imidazo [1, 2-a] pyridin-3- yl] phenyl} pyrrolidin-2-one as a pale yellow solid (114 mg, 31%): m/z [(ES+)] 372 [WHY]

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-Bromo-2-fluoroaniline, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; MERCK SHARP & DOHME LIMITED; WO2003/99816; (2003); A1;,
Bromide – Wikipedia,
bromide – Wiktionary