Tag: M.W=200-300

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 944718-31-4 as follows. Recommanded Product: 944718-31-4

5-bromo-1-methyl-1H-benzo[d][1,2,3]triazole (302.3 mg, 1.426 mmol),Benzophenone imine (342.5 mg, 1.890 mmol),t-BuONa (274.2 mg, 2.853 mmol),BINAP (87.8mg, 0.141mmol)And Pd2 (dba) 3 (131.4 mg, 0.1435 mmol)Dissolved in 1,4-dioxane (10 mL).The reaction mixture is at 100 ° C,Stir for 6 hours in a nitrogen atmosphere.After the reaction was completed, it was concentrated under reduced pressure.The residue was diluted with water (50 mL).The resulting mixture was taken with DCM and MeOHThe mixed solvent (10/1 (v/v), 80 mL × 3) was extracted.The combined organic phases were dried over anhydrous Na 2 SO 4 and filtered.The filtrate was concentrated under reduced vacuo afforded title crystallThe crude product was used directly in the next step without further purification.

According to the analysis of related databases, 944718-31-4, the application of this compound in the production field has become more and more popular.

Reference:
Patent; Guangdong Dongyangguang Pharmaceutical Co., Ltd.; Jiatuo Sciences Corporation; Xi Ning; Li Minxiong; Peng Ju; Li Xiaobo; Zhang Tao; Hu Haiyang; Chen Wuhong; Bai Changlin; Ke Donghua; Chen Peng; (217 pag.)CN109776522; (2019); A;,
Bromide – Wikipedia,
bromide – Wiktionary

Related Products of 1786-36-3, A common heterocyclic compound, 1786-36-3, name is (2-Bromo-1-fluoroethyl)benzene, molecular formula is C8H8BrF, 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.

Under a nitrogen atmosphere, nickel bromide (4.4 mg, 0.02 mmol),4,4′-dimethyl-2,2′-bipyridine (3.68 mg, 0.02 mmol),Tetrabutylammonium iodide (14.77 mg, 0.04 mmol) manganese powder (43.95 mg, 0.8 mmol),Add solvent NMP (0.5 mL) and stir well. Weigh 4-iodobenzaldehyde (46.40mg, 0.2mmol) in NMP (0.5mL),After dissolution, add (2-bromo-1-fluoroethyl) benzene (60.92 mg, 0.3 mmol) and mix well.The solution was transferred to a sealed tube. After sealing, the reaction was stirred in an oil bath at 80 C for 24 hours.Cool the reaction to room temperature, ether (5mL)Add an equal volume of saturated ammonium chloride solution to the diluted reaction solution.Filter through a diatomaceous sand core funnel, rinse with a small amount of ether, and collect the filtrate.The filtrate was extracted three times with diethyl ether, and the organic phases were combined (add internal standard dodecane,GC-MS determined crude yield). Dry over anhydrous sodium sulfate, filter, and remove the solvent by distillation under reduced pressure.After the residue was separated by silica gel column chromatography, the product was weighed, and the calculated yield was 46%.

The synthetic route of 1786-36-3 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Sichuan Qing Chemical University; Yang Yi; Luo Gen; Li Youlin; Tong Xia; He Mengmeng; Jiang Yan; Liu Yingle; Shu Yumei; Zheng Yubin; Lu Wenjie; Zhao Yanchuan; (22 pag.)CN110803977; (2020); A;,
Bromide – Wikipedia,
bromide – Wiktionary

Reference of 1074-24-4,Some common heterocyclic compound, 1074-24-4, name is 1,4-Dibromo-2,5-dimethylbenzene, molecular formula is C8H8Br2, 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.

In a 100 ml flask, with a magnetic stirrer, thermometer and coolant, in an inert atmosphere, the following were loaded, in order: 1 ,4-dibromo-2,5-dimethybenzene (Aldrich) (13.20 g; 50.0 mmoles) [dihalogenated acrylic compound having general formula (II) wherein Rn = methyl and X = bromine] and carbon tetrachloride (Aldrich) (1590 ml) and, after heating to reflux temperature, for 5 minutes, a bromine solution (Aldrich) (10.80 ml; 210 mmoles) in carbon tetrachloride (Aldrich) (50 ml) was added, by dripping: the reaction mixture obtained was maintained at reflux temperature, under stirring, and subjected to radiation with an incandescent lamp at 500 W (UV radiation emitted at 300 nm), for 4 hours. Subsequently, after cooling to room temperature (25°C), the reaction mixture obtained was placed in a 500 ml separator funnel: a concentrated aqueous solution of sodium bisulfite (NaHSOs) (Aldrich) (3 x 100 ml) and deionized water (Aldrich) (3 x 100 ml) was added to said reaction mixture and everything was extracted, obtaining an acidic aqueous phase and an organic phase. The entire organic phase (obtained by joining the organic phases deriving from the three extractions) was subsequently anhydrified on sodium sulfate (Aldrich) and evaporated. The residue obtained was recrystallized from ethyl acetate (Aldrich) (50 ml), obtaining 26.04 g of 1 ,4-dibromo-2,5- bis(dibromomethyl)benzene having formula (III) as white crystals (yield 89percent).

The synthetic route of 1074-24-4 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; ENI SPA; BIANCHI, Gabriele; PASINI, Dario; NITTI, Andrea; (67 pag.)WO2019/175367; (2019); A1;,
Bromide – Wikipedia,
bromide – Wiktionary

Related Products of 22385-77-9, 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. 22385-77-9, name is 1-Bromo-3,5-di-tert-butylbenzene, This compound has unique chemical properties. The synthetic route is as follows.

5.8 g (238.6 mmol) of magnesium turnings are initially introduced into a flask which has been dried by heating, and a solution of 73 g (271.1 mmol) of bromo-3,5-d-tert-butylbenzene in 400 ml of dry THF is slowly added dropwise so that the reaction solution constantly boils under reflux. When the addition is complete, the solution is heated under reflux for a further 2 h and then allowed to cool. 20 g (108.5 mmol) of cyanogen chloride in 400 ml of dry THF are initially introduced in a further flask and cooled to 0 C. The Grignard reagent is added dropwise at such a rate that an internal temperature of 20 C. is not exceeded. When the addition is complete, the reaction mixture is warmed at room temperature overnight. The reaction is stopped by addition of 500 ml of 1 N HCl solution with ice-cooling. The phases are separated, and the aqueous phase is rinsed a number of times with ethyl acetate. The organic phases are combined and dried using saturated NaCl solution, and the solvent is then removed in vacuo. Methanol is added to the pale-brown oil, and the mixture is heated under reflux. After cooling, the solid is filtered off with suction, washed with heptane and dried in vacuo, giving 23.6 g (48.0 mmol, 44% yield) of a colourless solid.

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

Reference:
Patent; MERCK PATENT GMBH; Koenen, Nils; Stoessel, Philipp; Hayer, Anna; Heil, Holger; Harbach, Philipp; (236 pag.)US9853228; (2017); B2;,
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. 327-51-5, name is 1,4-Dibromo-2,5-difluorobenzene, A new synthetic method of this compound is introduced below., Recommanded Product: 1,4-Dibromo-2,5-difluorobenzene

n-Butyl lithium (3.6 ml,7.7 mmol) was added drop wise to a solution of 1,4- dibromo-2,5-difluoro-benzene (2g, 7.35mmol) in dry ether at -78C under nitrogen atmosphere and the resulting mixture was stirred at -78C for 30 minutes. This was followed by the addition of DMF (0.85ml, 11.03mmol) in dry THF. The resultant was stirred at room temperature for 1 hour. The reaction was monitored by TLC (5% ethyl acetate in hexane). The reaction mixture was partitioned between ethyl acetate and saturated ammonium chloride. The organic layer was concentrated and purified by column chromatography on silica gel (2% ethyl acetate in hexane) to afford 600mg of the product (37% yield).1H NM (CDC13, 300 MHZ): delta 10.27-10.26 (d, 1H), 7.61-7.57 (t, 1H), 7.49- 7.44 (q, 1H)

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; NOVARTIS AG; BOCK, Mark Gary; GAUL, Christoph; GUMMADI, Venkateshwar Rao; SENGUPTA, Saumitra; WO2012/149413; (2012); A1;,
Bromide – Wikipedia,
bromide – Wiktionary

These common heterocyclic compound, 337915-79-4, name is 5-Bromo-N1-methylbenzene-1,2-diamine, 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. Safety of 5-Bromo-N1-methylbenzene-1,2-diamine

[000814j To a stirred solution of compound 1 (0.1 g, 1 eq) in DMF (5 mL),TEA ( 0.101 g, 2 eq) and 4-chlorobutanoyl chloride (0.06 1 g, 1 eq) was added at 0 C and stirred at room temperature for 12 h. The progress of the reaction was monitored by TLC. After completion of the reaction, the reaction mixture was evaporated under reduced pressure and the residue was basified using saturated sodium bicarbonate solution and extracted with ethyl acetate (2 X 20 mL). Combined organic extracts were washed with brine and dried over anhydrous sodium sulfate and evaporated under reduced pressure. The crude product was dissolved in acetic acid (5 mL) and was heated to 70 C for 18 h. The progress of the reaction was monitored by TLC. After completion of the reaction, the reaction mixture was evaporated under vacuum and residue was basified with saturated sodium bicarbonate solution and extracted with ethyl acetate (2 X 25 mL). Combined organic extracts were washed with brine and dried over anhydrous sodium sulfate and evaporated under reduced pressure. The crude product was purified by column chromatography on silica gel 100-200 mesh using 80% EtOAc-hexane to afford the title compound 2. LCMS (mlz): 289.00 (M + 1).

The synthetic route of 5-Bromo-N1-methylbenzene-1,2-diamine has been constantly updated, and we look forward to future research findings.

Reference:
Patent; BIOMARIN PHARMACEUTICAL INC.; BHAGWAT, Shripad; WANG, Bing; LUEDTKE, Gregory R.; SPYVEE, Mark; (490 pag.)WO2016/57834; (2016); A1;,
Bromide – Wikipedia,
bromide – Wiktionary

Reference of 3972-64-3, 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.

Compound 112a. To a solution of 1-bromo-3-(tert-butyl)benzene (0.2 g, 0.938 mmol, 1.0 equiv) in DMSO (10 mL) was added 4,4,4?,4?,5,5,5?,5?-octamethyl-2,2?-bi(1,3,2-dioxaborolane) (0.356 g, 1.41 mmol, 1.5 equiv), KOAc (0.184 g, 1.876 mmol, 2.0 equiv) and resulting reaction mixture purged with N2 gas for 10 minute, followed by the addition of Pd(PPh3)4 (0.055 g, 0.047 mmol. 0.05 equiv). The resulting reaction mixture was heated at 100 C. for overnight. Product formation was confirmed by LCMS. After the completion of reaction, the mixture was filtered through celite bed, washed with ethyl acetate (100 mL). Filtrate was concentrated under reduced pressure. The crude product obtained was purified by flash chromatography (hexane as an eluent) to obtain 2-(3-(tert-butyl)phenyl)-4,4,5,5-tetramethyl-1,3,2-dioxaborolane (0.230 g, 94.26% Yield) as an off-white solid. (0909) LCMS 261.3 [M+H]+ (0910) 1H NMR (400 MHz, DMSO-d6) delta7.67 (s, 1H), 7.57-7.45 (m, 2H), 7.32 (t, J=7.5 Hz, 1H), 1.44 (d, J=6.6 Hz, 1H), 1.39-1.23 (m, 9H), 1.23-1.04 (m, 12H)

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

Reference:
Patent; Praxis Biotech LLC; ALFARO, Jennifer; BELMAR, Sebastian; BERNALES, Sebastian; PUJALA, Brahmam; PANPATIL, Dayanand; BHATT, Bhawana; US2019/185451; (2019); A1;,
Bromide – Wikipedia,
bromide – Wiktionary

Electric Literature of 73918-56-6, A common heterocyclic compound, 73918-56-6, name is 2-(4-Bromophenyl)ethanamine, molecular formula is C8H10BrN, 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-Chloro-6-nitro-benzothiazol (200 mg, 0.93 [MMOL)] was placed in a 15 mi vial equipped with a stirring bar and septum. The vial was purged with argon and charged with DMF (1.0 [ML).] Diisopropyl-ethylamine (0.37 [ML,] 2 eq. ) was added resulting in a reddish solution. [2- (4-BROMO-PHENYL)-ETHYLAMINE] (186 mg, 1 eq. ) in DMF (1.0 [ML)] was added via syringe. The dark solution was then heated to 110 [C] for 30 minutes in an aluminum block. The mixture was cooled in an ice bath and diluted with water (10 [ML) WHILE] stirring vigorously. A dark precipitate formed. An additional 5 mi of water was added after stirring for 10 minutes and the product then collected by vacuum filtration. The product was washed with distilled water (2 x 10 ml) and dried under suction. The sample was dried under high vacuum (0.8 torr, 110 [C,] 20 hours) to give a solid (198 mg, 61%). %).’H NMR [(CDC13)] 8 : 8.5 (s, [1H),] 8.21 (br d, [1H,] J=7.7 Hz), 7.48 m (3H), 7.10 (d, 2H, J=7.7 Hz), 5. 68 (br s, 1H), 3.75 (br t, 3H), 2.99 [(BR T, 3H).]

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; MCR RESEARCH INC.; WO2004/14885; (2004); A1;,
Bromide – Wikipedia,
bromide – Wiktionary

Reference of 2606-51-1, These common heterocyclic compound, 2606-51-1, name is 5-(Bromomethyl)benzo[d][1,3]dioxole, 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.

1.1 equiv. of 5-(bromomethyl)-1,3-benzodioxole, 1 equiv. ofnoscapine were taken in 3 ml of toluene in a 25 ml round bottom flaskand at 60 C for 20 h on a continuous stirring in an oil bath. After thecompletion of reaction, toluene was decanted and remaining solid residuewas washed with ethyl acetate to remove the unreacted part(3 × 10 ml). Chloroform was added to dissolve the solid productfollowed by evaporation on a vacuum rotary evaporator to obtain 3 asthe solid ionic liquid product.

The synthetic route of 2606-51-1 has been constantly updated, and we look forward to future research findings.

Reference:
Article; Sehrawat, Hitesh; Kumar, Neeraj; Tomar, Ravi; Kumar, Loveneesh; Tomar, Vartika; Madan, Jitender; Dass, Sujata K.; Chandra, Ramesh; Journal of Molecular Liquids; vol. 302; (2020);,
Bromide – Wikipedia,
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89359-54-6, name is 9-Bromo-1-nonene, 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. Product Details of 89359-54-6

Example 37 This example illustrates the synthesis of 1-(8-Nonenyl)-3,7-dimethylxanthine (CT1550). A mixture of theobromine (17.64 g, 98 mmol) and sodium hydride (2.35 g, 98 mmol) in dimethylsulfoxide (250 ml) was stirred for 15 min. After addition of 9-bromo-1-nonene (Alfebro, 20.0 g, 98 mmol) stirring was continued at ambient temperature for 3 days. The reaction mixture was then poured into water (300 ml) and extracted with dichloromethane (4*200 ml). The combined organic layers were washed with saturated aqueous salt solution (2*150 ml) and dried over sodium sulfate. The solvent was evaporated under vacuum to give a thick oil. After cooling a solution of the oil in a minimum of dichloromethane and ether, 1-(8-nonenyl)-3,7-dimethylxanthine (CT1550) (24.34 g, 77.5 mmol, 99% yield) formed as white crystals.

The synthetic route of 89359-54-6 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Cell Therapeutics, Inc.; US5521315; (1996); A;,
Bromide – Wikipedia,
bromide – Wiktionary