Tag: M.W=200-300

Related Products of 102169-44-8,Some common heterocyclic compound, 102169-44-8, name is 4-Bromo-5-methylbenzene-1,2-diamine, molecular formula is C7H9BrN2, 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.

B. 6-Bromo-1,4-diethyl-7-methyl-1,4-dihydro-quinoxaline-2,3-dione (Compound 24B); Compound 24A (160 mg) in 1 mL of diethyl oxalate was heated in microwave at 140 C. for 30 min. Reaction was then cooled to rt, diluted with hexanes and resulting dark brown solid (164 mg, 81%) was collected by filtration. Solution of above intermediate (164 mg, 1 eq.) and ethyl iodide (0.52 mL, 10 eq.) in 3 mL of anhydrous DMSO was cooled on ice and crushed into powder KOH (144 mg, 4.0 eq.) was added slowly. Reaction was stirred on ice for 1 hour and at rt for another hour. Reaction was then partitioned between CH2Cl2 and water. The organic layer was separated, dried over Na2SO4, filtered and the solvent was removed in vacuo. Crude was purified by column chromatography (40:60 hexane/EtOAc) to obtain 157 mg (78 %) of product. MS (electrospray): mass calculated for C13H15BrN2O2, 311.17; m/z found 312.2, [M+H]+.

The synthetic route of 102169-44-8 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Lagu, Bharat; Lebedev, Rimma; Pio, Barbara; US2007/78129; (2007); A1;,
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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. 327-52-6, name is 1-Bromo-2,4,5-trifluorobenzene, A new synthetic method of this compound is introduced below., category: bromides-buliding-blocks

116.05g trifluorobromobenzene and 400ml tetrahydrofuran were added to a clean flask. The resulting mixture was cooled to -10 to -5C, and then 864ml (0.7mol) methyl magnesium bromide was added thereto dropwisely. The mixture was stirred for 1 hour for use. 23.5g (S)-methyl 3-(benzyloxycarbonylamino)-4-oxo n-butyrate was dissolved in 300ml THF, and added dropwisely to the mixture mentioned above and kept at this temperature for 3 hours after completion of the addition. 400ml solution of ammonium chloride was added dropwisely. Layers were separated. The aqueous layer was extracted with tetrahydrofuran (200ml X 2). The organic layer was dried and concentrated to get 31.4g (3S)-methyl 3-(benzyloxycarbonylamino)-4-hydroxy-4-(2,4,5-trifluorophenyl) butyrate (yield: 78.5%).

The synthetic route of 327-52-6 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Zhejiang Jiuzhou Pharmaceutical Co., Ltd.; EP2481722; (2012); A1;,
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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. 6274-57-3, name is 1-(4-Bromophenyl)-N,N-dimethylmethanamine, A new synthetic method of this compound is introduced below., SDS of cas: 6274-57-3

To a solution of (4-bromophenyl)-N,N-dimethylmethanamine (4.26 g, 20.00 mmol, 1.00 equiv) in tetrahydrofuran (60 mL) maintained under nitrogen at -78C was added in 30 min a 2.5M solution of n-butyllithium (8.8 mL, 1.10 equiv) in hexane dropwise with stirring. The resulting solution was stirred at -78C for 2 h. Sulfur dioxide gas was then bubbled into the solution at -78C for 1 h. Ether (200 mL) was added and the precipitate was collected by filtration. The solid was washed with ether and dried in vacuum to give 4 g (98%) of lithium 4-((dimethylamino)methyl)benzenesulfinate as a yellow solid.

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; THE BOARD OF TRUSTEES OF THE LELAND STANFORD JUNIOR UNIVERSITY; AUCKLAND UNISERVICES LIMITED; RUGA CORPORATION; GIACCA, Amato; LAI, Edwin; RAZORENOVA, Olga; CHAN, Denise; HAY, Michael, Patrick; BONNET, Muriel; SUN, Connie; TABIBIAZAR, Ray; YUEN, Po-wai; WO2013/155338; (2013); A2;,
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Electric Literature of 57946-63-1, 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 57946-63-1 as follows.

EXAMPLE 6 4-(2-Bromo-4-trifluoromethyl-phenylcarbamoyl)-piperidine-1-carboxylic acid tert-butyl ester Piperidine-1,4-dicarboxylic acid mono-tert-butyl ester (4.90 g, 21.00 mmol) was dissolved in dry methylene chloride (30 mL) and dry pyridine (4.30 mL). To the reaction mixture was then added thionyl chloride (3.00 g, 25.20 mmol) under nitrogen atmosphere and the reaction mixture was stirred at room temperature for 30 minutes. To the reaction mixture was then added successively, under nitrogen atmosphere, 2-bromo-4-trifluoromethyl-phenylamine (5.60 g, 23.50 mmol), dry triethylamine (7.43 g, 73.5 mmol), dry methylene chloride (38 mL), 4-(dimethylamino)pyridine (0.26 g, 2.18 mmol) and the reaction mixture was stirred at room temperature for 24 hours. The reaction mixture was then partitioned with aqueous 2N HCl and tert-butyl methyl ether. The organic layer was washed with aqueous 2N HCl, aqueous NaHCO3, brine, dried with Na2SO4, filtered and the solvent evaporated in vacuo to yield a crude oil. The crude oil was purified via flash chromatography (30percent ethyl acetate/hexanes) to yield the title compound as an oil. 1H NMR (300 MHz, CDCl3) delta 8.5 (1H, d, J=9 Hz), 7.6 (1H, bs) 7.5 (1H, d, J=7.0 Hz), 7.3 (1H, d, J=8 Hz), 4.18 (2H, m), 2.8 (2H, m), 1.9 (2H, d), 1.8 (2H, m), 1.47 (9H, s) MS (ES+) m/z 475.0 (MNa)+

According to the analysis of related databases, 57946-63-1, the application of this compound in the production field has become more and more popular.

Reference:
Patent; Battista, Kathleen A.; Bignan, Gilles C.; Connolly, Peter J.; Liu, Jessica J.; Middleton, Steven A.; Orsini, Michael J.; US2007/112016; (2007); A1;,
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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. 22385-77-9, name is 1-Bromo-3,5-di-tert-butylbenzene belongs to bromides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below. Product Details of 22385-77-9

The title compound 1e was prepared according to a proceduredescribed by Zhu et al.31 Where 1-bromo-3,5-di-tert-butylbenzene(2.50 g, 9.30 mmol), CuI (0.177 g, 0.93 mmol), NaN3 (1.21 g,18.57 mmol), l-proline (0.321 g, 2.74 mmol) and NaOH (0.11 g,2.79 mmol) were added to EtOH:H2O (7:3, 20 mL) and heated to95 C in a sealed tube for 23 h. The reaction mixture was thenadded water (30 mL) and extracted with EtOAc (3 30 mL). Dryingover MgSO4 and evaporation under reduced pressure yielded a yellowoil, which then was purified using flash column chromatography(pentane), affording 1e as a colorless oil (0.725 g, 3.13 mmol,34percent). 1H NMR spectra coincided with previously reported data.441H NMR (400 MHz, CDCl3): d 7.20 (t, 1H, J = 1.5 Hz, HPh-4), 6.86(d, 2H, J = 1.6 Hz, HPh-2 and HPh-6), 1.31 (s, 18H, 2 t-Bu).

The synthetic route of 22385-77-9 has been constantly updated, and we look forward to future research findings.

Reference:
Article; Bakka, Thomas A.; Str°m, Morten B.; Andersen, Jeanette H.; Gautun, Odd R.; Bioorganic and Medicinal Chemistry; vol. 25; 20; (2017); p. 5380 – 5395;,
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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. 615-59-8, name is 1,4-Dibromo-2-methylbenzene, A new synthetic method of this compound is introduced below., HPLC of Formula: C7H6Br2

In a dry 500ml round-bottomed flask (equipped with a water-cooled condenser, a gas outlet, and a stir bar) palladium acetate (0.449g, 2.00mmol), tri(o-tolyl)phosphine (1.22g, 4.00mmol), and potassium tert-butoxide (1 1 .2g, lOOmmol) were combined. The apparatus was sealed, purged with nitrogen, and 60mL anhydrous toluene was added. To the resulting suspension 3-S-methylmorpholine (4.04g, 40.0mrnoi), and 2,5-dibromotoluene (12.5g,

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; ATHENEX, INC.; SMOLINSKI, Michael P.; NASIEF ABDEL-SAYED, Nader N.; HANGAUER, JR., David G.; (197 pag.)WO2018/31988; (2018); A1;,
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Reference of 51554-93-9,Some common heterocyclic compound, 51554-93-9, name is 1-Bromo-4-octylbenzene, molecular formula is C14H21Br, 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.

To the solution of 1 -bromo-4-octylbenzene (3.733 g; 12.48 mmol;) in dry THF (20.0 cm3) at -78 C was added n-BuLi (5.0 cm3; 12.5 mmol). The mixture was stirred at -78 C for 2 hours to yield a pale-yellow clear solution. The solid of diethyl 2,5-di(thieno[3,2-b]thiophen-2-yl)terephthatate (3) (1.30 g; 2.60 mmol) was added in one portion and the mixture (a yellow suspension) was stirred at -78 C for 20 minutes. The cooling bath was removed and the mixture was stirred at 22 C for 50 hours to yield a deep yellow clear solution. Saturated ammonium chloride solution (50 cm3) was added and the mixture was stirred for 15 minutes. The orange oil was taken into diethyl ether (2 x 50 cm3). The solvent was concentrated till a yellow solid started crashing out. Methanol (50 cm3) was added to the residue and the precipitate was collected by suction filtration and washed with methanol.The solid was dissolved in dry DCM (50 cm3) andBF3 etherate (1.0 cm3; 8.10 mmol) was added. The blue clear solution was stirred at 22 C for 1 hour followed by the addition of methanol (150 cm3). The yellow precipitate was suction filtered off and washed with methanol. The solid was further purified by flash column chromatography on silica (9:1 petroleum ether 40- 60-chloroform) to yield the productas a bright-yellow solid (1.06 g, 36%). *H-NMR (CDCI3, 300 MHz): delta= 0.86 (t, J = 6.7 Hz, 6H), 1.25 (m, 20H), 1.58 (m, 4H), 2.54 (t, J = 7.8 Hz, 4H), 7.07 (d, J = 8.3 Hz, 4H), 7.18 (d, J = 8.3 Hz, 4H), 7.25 (d, J = 5.2 Hz, 1H), 7.27 (d, J = 7.2 Hz, 1H), 7.50 (s, 1H).

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 1-Bromo-4-octylbenzene, its application will become more common.

Reference:
Patent; MERCK PATENT GMBH; WANG, Changsheng; TIERNEY, Steven; D’LAVARI, Mansoor; NANSON, Lana; WO2013/10614; (2013); A2;,
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Synthetic Route of 698-00-0, A common heterocyclic compound, 698-00-0, name is 2-Bromo-N,N-dimethylaniline, 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.

General procedure: TMSCN (0.15 mL, 1.0 mmol) was added to a stirred mixture of PIFA (430 mg,1.0 mmol) and 3.0 mL of DCE at room temperature. After 40 min, Na2SO4(36 mg, 0.25 mmol) and tertiary amine (0.5 mmol) were then added to themixture successively and reacted for overnight. Subsequently,the mixture was poured into aqueous NaHCO3 solution and Na2S2O3solution and extracted with dichloromethane. The organic layer was washedwith brine, dried over sodium sulfate and concentrated in vacuo. Purificationby column chromatography on silica gel produced alpha-aminonitriles.

The synthetic route of 698-00-0 has been constantly updated, and we look forward to future research findings.

Reference:
Article; Shen, Hang; Zhang, Xiaohui; Liu, Qing; Pan, Jing; Hu, Wen; Xiong, Yan; Zhu, Xiangming; Tetrahedron Letters; vol. 56; 41; (2015); p. 5628 – 5631;,
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Synthetic Route of 185122-74-1, 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. 185122-74-1, name is 5-Bromo-2,3-dihydro-1H-inden-1-amine belongs to bromides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

5-bromo-2,3-dihydro-lH-inden-l -amine (2.2 g, 10.4 mmol) andSodium bicarbonate (2.6 g, 31.2 mmol)Suspended in acetonitrile (100 mL)The mixture was cooled to 0 C,To this was added Boc anhydride (3.4 mL, 15.6 mmol).The reaction mixture was stirred at room temperature overnight and concentrated under reduced pressure.The residue was taken up in ethyl acetate (100 mL) and the resulting solution was washed with water (50 mL x 2), dried over anhydrous sodium sulfate, filtered and concentrated under reduced pressure.The residue was purified by silica gel column chromatography (petroleum ether / ethyl acetate (v / v) = 20/1)The title compound was obtained as a white solid (3.3 g, 100%).

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-2,3-dihydro-1H-inden-1-amine, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; Guangdong Dongyangguang Pharmaceutical Co., Ltd.; Jiatuo Sciences Corporation; Xi Ning; Wang Ruyong; Wang Liang; (112 pag.)CN104016979; (2017); B;,
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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 18599-22-9 as follows. Safety of 4-Bromo-3,3,4,4-tetrafluorobut-1-ene

To a stirred solution of silver acetate (10 mg, 0.060 mmol) in glacial acetic acid (20 mL) at reflux temperature was added zinc powder (10 g, 153 mmol) in one portion, and the whole was stirred at that temperature for additional 30 seconds. After refluxing for 30 seconds, the flask was cooled by dipping in an ice-bath. The Zn-Ag couple formed was separated by vacuum filtration in the open-air, which was washed with Et2O several times, followed by drying under reduced pressure. The Zn-Ag couple separated was stored at room temperature under Ar atmosphere. See Figure S1 Preparation of CH2=CHCF2CF2ZnBr in DMF (2-Zn) In a two-necked round-bottomed flask, equipped with a teflon-coated stirrer bar, was placed Zn-Ag couple (0.66 g, 10 mmol) in DMF (5.0 mL). To the suspension was slowly dropwise added 4-bromo-3,3,4,4-tetrafluorobut-1-ene (1, 1.0 g, 5.0 mmol) at 0 C and the whole was stirred at that temperature for 30 min. The resultant was subjected to a short pad of celite and washed by Et2O three times. The filtrate was concentrated in vacuo to give the corresponding organozinc reagents 2-Zn in 86% NMR yield as a 0.70 M DMF solution (1,1,2,2-Tetrafluorobut-3-en-1-yl)zinc bromide in DMF (2-Zn) Yield: 86% (determined by 19F NMR); 19F NMR (CDCl3): 112.10 (brs, 2F, CF2CH), 120.23 (brs, 2F, CF2Zn).

According to the analysis of related databases, 18599-22-9, the application of this compound in the production field has become more and more popular.

Reference:
Article; Tamamoto, Ken; Yamada, Shigeyuki; Konno, Tsutomu; Beilstein Journal of Organic Chemistry; vol. 14; (2018); p. 2375 – 2383;,
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