Tag: M.W=100-200

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. 1647-26-3, name is 1-Bromo-2-cyclohexylethane, This compound has unique chemical properties. The synthetic route is as follows., Recommanded Product: 1647-26-3

1-(2-Chloro-phenyl)-3-cyclohexyl-propan-1-one 15.57 g (640 mmole) Magnesium turnings were placed in a 1 l-roundbottom flask equipped with a dropping funnel and a reflux condenser, and 50 ml of THF were added. The magnesium was etched slightly with a few crystals of iodine and then 2 g of (2-bromo-ethyl)-cyclohexane were added and the mixture was heated locally. After the start of the Grignard-formation the rest of the (2-bromo-ethyl)-cyclohexane in 350 ml of THF (112.65 g in total, 589 mmole) were added within a period of 20 min. The mixture was refluxed for 1.5 h and then cooled to room temperature. In a separate 2 l-roundbottom flask 70.5 g (513 mmole) of 2-chloro-benzonitrile and 156 mg (0.16 mole %) copper(I)iodide were dissolved in 130 ml of THF. The Grignard-solution was added dropwise over a period of 30 min and the reaction mixture was refluxed for 3 h. After standing overnight at room temperature, a mixture of 190 ml water and 127 ml concentrated hydrochloric acid were added very carefully, causing a strongly exothermic reaction. The mixture was stirred at 50 C. for 1 h and the layers were separated. The aqueous layer was extracted twice with 150 ml of toluene each. The combined organic layers were washed twice with 2 M sulphuric acid, once with a saturated sodium bicarbonate solution and once with a saturated sodium chloride solution. After drying over magnesium sulphate the solvent was evaporated in vacuo to yield 133.5 g (quant.) of the desired phenone as slightly brown oil. 1H-NMR (400 MHz, CDCl3): delta=7.41-7.14 (m, 4H, aromatic), 2.91 (t, 2H, COCH2), 1.71-1.55, 1.28-1.10, 0.93-0.85 (3*m, 13H) ppm.

According to the analysis of related databases, 1647-26-3, the application of this compound in the production field has become more and more popular.

Reference:
Patent; Lammus Novolen Technology GmbH; US8299287; (2012); B2;,
Bromide – Wikipedia,
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Reference of 626-88-0,Some common heterocyclic compound, 626-88-0, name is 1-Bromo-4-methylpentane, molecular formula is C6H13Br, 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.

Step 1: 2-(4-methylpentyl)-1H-isoindole-1,3(2H)-dione To a solution of 1-bromo-4-methylpentane (5.0 g, 0.030 mol) in DMF (20 mL) was added potassium phthalimide (5.9 g, 0.032 mol) in one portion at room temperature. After stirring at room temperature of 1 hr, the mixture was heated at 55 C. for 16 hr. Chloroform (30 mL) was added to the reaction mixture and the resulting mixture was poured into water (100 mL). The aqueous phase was extracted with chloroform and the combined organic phase was washed with 0.25 M NaOH (aq) and water. The organic phase was dried (Na2SO4), filtered and concentrated in vacuo to give 2-(4-methylpentyl)-1H-isoindole-1,3(2H)-dione as a pale yellow oil. (M+H) 232, 2.80 min. (LC/MS method A).

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-methylpentane, its application will become more common.

Reference:
Patent; IGNAR, DIANE MICHELE; US2010/113512; (2010); A1;,
Bromide – Wikipedia,
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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 766-81-4 as follows. SDS of cas: 766-81-4

EXAMPLE 26; Preparation of 2-Amino-5-(5-chloro-2-methylthien-3-yl)-3-methyl-5-(3-pyrimidin-5-ylphenyl)-3,5-dihydro-4H-imidazol-4-one; Step a); Preparation of Compound 14; A mixture of 13 (3.17 g, 12.3 mmol), 3-bromophenylacetylene (2.44 g, 13.5 mmol; see MEC00775; dated Aug. 15, 2003), bis(triphenylphosphine)palladium(II) chloride (0.258 g, 0.360 mmol), copper(I) iodide (0.046 g, 0.240 mmol) and triethylamine (3.70 g, 36.8 mmol) in dimethylformamide (60 mL) was stirred at room temperature for 1.5 h. The mixture was diluted with ethyl acetate (300 mL), washed with water (2¡Á100 mL), brine (3¡Á100 mL), dried over sodium sulfate, filtered, and concentrated. The crude material was purified by flash chromatography (silica, hexanes) to afford 14 as a yellow oil, which was a mixture of product and an unidentified by-product (which was removed during purification in the following step): APCI MS m/z 311 [C13H8BrClS+H]+.

According to the analysis of related databases, 766-81-4, the application of this compound in the production field has become more and more popular.

Reference:
Patent; Wyeth; US2007/4786; (2007); A1;,
Bromide – Wikipedia,
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Reference of 1647-23-0,Some common heterocyclic compound, 1647-23-0, name is 1-Bromo-3,3-dimethylbutane, molecular formula is C6H13Br, 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.

Into a 1 L round bottom flask equipped with a dropping funnel and a reflux condenser, 14.1 g (580 mmol) of shaved magnesium was added and 60 ml THF was added. Magnesium was etched slightly with a few iodine crystals, then 2 g of 1-bromo-3,3-dimethyl-butane was added and the mixture was locally heated. After the onset of Grignard formation, the remainder of 1-bromo-3,3-dimethyl-butane (total 88.1 g, 553 mmol) in 350 ml of THF was added within 20 minutes. The mixture was refluxed for 1.5 hours and then cooled to room temperature. In a separate 2 L round bottom flask, 63.9 g (464 mmol) of 2-chloro-benzonitrile and 141 mg (0.16 mol%) of copper (I) iodide were dissolved in 265 ml of THF. The Grignard solution was added dropwise over 30 minutes and the reaction mixture was refluxed for 3 hours. After standing overnight at room temperature, a mixture of 190 ml of water and 127 ml of concentrated hydrochloric acid was added very carefully to produce a strongly exothermic reaction. The mixture was stirred at 50 C. for 1 hour and the layers were separated. The aqueous layer was extracted twice with 150 ml each of toluene. The combined organic layers were washed twice with 2 M sulfuric acid, once with saturated sodium bicarbonate solution and once with saturated sodium chloride solution. After drying over magnesium sulfate, the solvent was evaporated in vacuo to give 103.8 g (quantitative) of the desired phenone as a slightly brown oil.

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-3,3-dimethylbutane, its application will become more common.

Reference:
Patent; LUMMUS NOVOLEN TECHNOLOGY GMBH; (91 pag.)JP6196581; (2017); B2;,
Bromide – Wikipedia,
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Reference of 4333-56-6, These common heterocyclic compound, 4333-56-6, name is Bromocyclopropane, 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.

To a stirred suspension of magnesium turnings (300 mg, 12.3 mmol) in THF (2.0 mL) was added commercially available cyclopropyl bromide (0.800 mL, 9.99 mmol) in THF (17.2 mL) dropwise at room temperature over 30 min. During this operation, the reaction continued refluxing without heating. After the addition of the halide was completed, the mixture was stirred at room temperature for 5 h. The concentration of this solution of 40 was determined by titration as shown below. Titration. After an exactly 0.150-mL aliquot of the Grignard solution of 40 was quenched with an exactly known volume (0.250 mL) of a 1.000 M HCl standard solution (purchased from Yoneyama Yakuhin Kogyo, Co., Ltd. (Japan)), the mixture was then titrated with a 0.500 M NaOH standard solution (purchased from Yoneyama Yakuhin Kogyo, Co., Ltd. (Japan)) (0.352 mL) with methyl orange as an indicator to determine its concentration to be 0.49 M. Thus, the yield of the Grignard reagent was 98% based on the halide. In several runs, the Grignard concentrations usually fell within a range between 0.48 and 0.51 M.

Statistics shows that Bromocyclopropane is playing an increasingly important role. we look forward to future research findings about 4333-56-6.

Reference:
Article; Sugano, Goshi; Kawada, Kojiro; Shigeta, Masayuki; Hata, Takeshi; Urabe, Hirokazu; Tetrahedron Letters; vol. 60; 13; (2019); p. 885 – 890;,
Bromide – Wikipedia,
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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. 1073-06-9, name is 1-Bromo-3-fluorobenzene belongs to bromides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below. SDS of cas: 1073-06-9

General procedure: A mixture of a fluorinated aryl halide (2.0 mmol), a carbazole (0.5 mmol), and a base (2.0 mmol) in solvent (2 mL) was allowed to react under air atmosphere. The reaction mixture was heated to the specified temperature for 24 h. After reaction completion, the mixture was added to brine (15 mL) and extracted with CH2Cl2 (3 ¡Á 15 mL). The combined extract was concentrated under reduced pressure and the product was isolated by short chromatography on a silica gel (200-300 mesh) column.

The synthetic route of 1073-06-9 has been constantly updated, and we look forward to future research findings.

Reference:
Article; Wang, Lei; Ji, Enhui; Liu, Ning; Dai, Bin; Synthesis; vol. 48; 5; (2016); p. 737 – 750;,
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Electric Literature of 766-46-1, The chemical industry reduces the impact on the environment during synthesis 766-46-1, name is 2′-Bromophenylacetylene, I believe this compound will play a more active role in future production and life.

General procedure: To a solution of sulfonyl azides 1 (0.6 mmol), o-bromo-phenylacetylenes 2 (0.5 mmol), aromatic amines 3 (0.55 mmol), and CuI (0.05 mmol) in DMSO (2 mL) in Schlenk tube was added TEA (0.5 mmol) slowly via a syringe. The reaction solution was stirred at room temperature under N2 for 2 h. The solution was then added to CuI (0.05 mmol), K2CO3 (1 mmol), and l-proline (0.2 mmol), and the mixture was stirred at 60 C under N2 for 4 h. The reaction mixture was partitioned between ethyl acetate and saturated aq NH4Cl, the organic layer was washed with brine, dried over Na2SO4, and concentrated in vacuo. The residue was purified by column chromatography on silica gel with petroleum ether and ethyl acetate (6:1 to 9:1).

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, 2′-Bromophenylacetylene, other downstream synthetic routes, hurry up and to see.

Reference:
Article; Jin, Hongwei; Zhou, Bingwei; Wu, Zhi; Shen, Yang; Wang, Yanguang; Tetrahedron; vol. 67; 6; (2011); p. 1178 – 1182;,
Bromide – Wikipedia,
bromide – Wiktionary

Reference of 6911-87-1, 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. 6911-87-1 name is 4-Bromo-N-methylaniline, 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.

37.0 mg (0.2 mmol) of N-methyl-4-bromoaniline, 81.2 mg of ethyl bromodifluoroacetate (0.4 mmol), 2.5 mg (0.02 mmol) of cuprous acetate, 19.1 mg (0.04 mmol) of X-phos, 32.7 mg (0.2 mmol) of cesium carbonate were added to 2 mL of DMF solvent. The reaction was carried out at 110 C for 12 hours, after the reaction was completed, it was cooled, filtered, and the filtrate was evaporated. The solvent was removed and the residue was chromatographed on silica gel. It was washed with a mixed solution of petroleum ether and ethyl acetate in a volume ratio of 8:1. The effluent was collected according to the actual gradient, detected by TLC, and the effluent containing the product was combined. The solvent was distilled off by a rotary evaporator. Drying in vacuo to give the yellow liquid -N-(4-bromophenyl)-N-methylformamide 26.0 mg, yield 61%.

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

Reference:
Patent; Wenzhou University; Zhang Xiaohong; Li Xiaofang; Zhang Xingguo; (15 pag.)CN108774147; (2018); A;,
Bromide – Wikipedia,
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2550-36-9, name is (Bromomethyl)cyclohexane, 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. HPLC of Formula: C7H13Br

Step 1 : Ethyl 1-(cvclohexylmethyl)-5-methyl-1 H-pyrrole-2-carboxylate (1a)A solution of ethyl 5-methyl-1 –pyrrole-2-carboxylate (15.0 g, 98.0 mmol), (bromo- methyl)cyclohexane (17.6 g, 100 mmol) and K2C03 (41.4 g, 300 mmol) in dry DMF (150 mL) was stirred at 50C overnight, then cooled to rt and filtered. To the filtrate was added NaH (12.0 g, 60%, 300 mmol) slowly. Then the mixture was stirred overnight at 50C. The reaction mixture was quenched with water and extracted with EA twice. The combined organic phases were washed with water (3 x) and brine (2 x), dried over Na2S04l filtered, concentrated and purified by CC (EA/PE = 1/20) to give compound 1a (19.9 g, 82%) as a white solid.

The synthetic route of 2550-36-9 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; PHENEX PHARMACEUTICALS AG; STEENECK, Christoph; KINZEL, Olaf; GEGE, Christian; KLEYMANN, Gerald; HOFFMANN, Thomas; WO2012/139775; (2012); A1;,
Bromide – Wikipedia,
bromide – Wiktionary

Application of 556-96-7, 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. 556-96-7, name is 1-Bromo-3,5-dimethylbenzene belongs to bromides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

General procedure: Heck coupling reactions were carried out in air. In a typicalexperiment, an oven-dried, sealed tube equipped with amagnetic stir bar was charged with aryl bromide (0.1 mmol),styrene (0.12 mmol) and a base (0.12 mmol). The catalyst solution(0.0004 mmol catalyst in 2.0 ml solvent) was then added.The reaction mixture was placed in a silicon oil bath at 140Cand stirred. After the required reaction time, the mixture wasallowed to cool to room temperature, dilutedwith CH2Cl2, andwashed withHCl aqueous solution and brine. The organic phasewas separated and dried over Na2SO4, and the solventwas evaporated.The residue was chromatographed on silica gel using anethyl acetate/hexane (1:5) mixture as eluent. Conversion percentageswere determined fromthe solution by GC analysis, andisolated yields, which were characterized by 1H and 13C NMR,determined by GC based on ArBr

The synthetic route of 1-Bromo-3,5-dimethylbenzene has been constantly updated, and we look forward to future research findings.

Reference:
Article; Altan, Orhan; Serinda?, Osman; Say?n, Koray; Karaka?, Duran; Phosphorus, Sulfur and Silicon and the Related Elements; vol. 191; 7; (2016); p. 993 – 999;,
Bromide – Wikipedia,
bromide – Wiktionary