Month: May 2021

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. 72635-78-0, name is 3-Amino-4-bromobenzonitrile belongs to nitriles-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below. SDS of cas: 72635-78-0

To R27 (25.0 g, 111 mmol) in acetonitrile (750 mL) is added MeI (15 mL, 241 mmol) and K2CO3 (60.0 g, 434 mmol) and the reaction mixture is stirred at 60 C. for 2 h. The reaction mixture is filtered and concentrated. Water and ethyl acetate are added to the residue. The organic layer is extracted twice with water, dried over MgSO4 and concentrated. Yield 56%. For I-12.1.1, I-12.1.2, I-12.1.3, I-12.1.5, I-12.1.7 and I-12.1.8 sodium hydride and DMF is used instead of potassium carbonate and ACN. For I-12.1.3, I-12.1.7 and I-12.1.8 the reaction temperature is r.t.

The synthetic route of 72635-78-0 has been constantly updated, and we look forward to future research findings.

Some common heterocyclic compound, 191014-55-8, name is 4-Fluoro-2-methoxybenzonitrile, molecular formula is C8H6FNO, 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 4-Fluoro-2-methoxybenzonitrile

To a solution of 1.34 g of [4-(3-benzyloxy-propyl)-2-(4-trifluoromethyl-phenyl)-thiazol-5- yl]-methanol in 20 ml_ of dimethylformamide at 00C was added 158 mg of a 60% suspension of sodium hydride in mineral oil. The resulting mixture was stirred for 10 minutes at 00C then 497 mg of 4-fluoro-2-methoxybenzonitrile were added. After stirring for 30 minutes at 00C, the temperature was allowed to warm up to room temperature and the reaction mixture was stirred until completion. The solvent was removed under reduced pressure and dichloromethane/water were added to the residue. The organic layer was separated and the aqueous layer extracted three times with dichloromethane. The combined organic extracts were washed with brine, dried over magnesium sulfate, filtered, and concentrated under reduced pressure to give 1.82 g of crude product as a yellow oil. A 1/1 solution of heptane/ diisopropyl ether was added to the residue and the solidified product was filtered off to provide a first crop of 1.26 g of desired product. The mother liquor was concentrated and purified by column chromatography on silica gel (heptane 60/ ethyl acetate 40) to give an additional 110 mg. The two fractions were combined to obtain 1.37 g of 4-[4-(3-benzyloxy-propyl)-2- (4-trifluoromethyl-phenyl)-thiazol-5-ylmethoxy]-2-methoxy-benzonitrile. C29H25F3N2O3S (538.59), MS(ESI): 539 (M+H+).

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 191014-55-8, its application will become more common.

Application of 143879-78-1, 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 143879-78-1 as follows.

Methyl 1 -methyl-4-[ [(1 S)-2,2,2-trifluoro- i-methyl-ethyl] sulfamoyl]pyrrole-2-carboxylate (0.7 g, 2.23 mmol) was dissolved in THF (10 mL) under nitrogen. To this was added 3-amino-2,6- difluorobenzonitrile (0.45 g, 2.9 mmol) and the mixture was cooled in an ice-water bath while stirred under nitrogen. To this was added drop wise lithium bis(trimethylsilyl)amide 1M intoluene (6.68 mL, 6.68 mmol) over a period of 10 minutes. The resulting mixture was stirred for1 hour while cooling was continued. The mixture was quenched with saturated ammonium chloride (25 mL) and the resulting mixture was extracted using EtOAc (3 x 25 mL). The combined extracts were washed with brine (20 mL), dried on Na2SO4, filtered and concentrated in vacuo. The obtained residue was dissolved in 2 mL dichloromethane and this was loaded on a dry silica plug. This was purified by column chromatography using gradient elution fromheptane to EtOAc. (100:0 to 0:100). The desired fractions were collected and concentrated in vacuo yielding a powder. This powder was recrystallized out of MeOH/water. The obtained crystals were collected on a filter, rinsed with water followed by diisopropylether and dried in a vacuo at 55C for 24 hours resulting in N-(3-Cyano-2,4-difluorophenyl)-1-methyl-4-{[(1S)- 2,2,2-trifluoro- 1 -methylethyl] sulfamoyl} -1 H-pyrrole-2-carboxamide (563 mg) as a powder.Method A: Rt: 1.75 mm mlz: 435.0 (M-H) Exact mass: 436.06. ?H NMR (400 MHz, DMSO-d6) oe ppm 1.09 (d, J=6.8 Hz, 3 H), 3.80 – 4.06 (m, 4 H), 7.36 (d, J2.0 Hz, 1 H), 7.40 – 7.51 (m, 1 H), 7.66 (d, J=1.5 Hz, 1 H), 7.85 – 8.02 (m, 1 H), 8.54 (br. s, 1 H), 10.14 (br. s, 1 H).

According to the analysis of related databases, 143879-78-1, the application of this compound in the production field has become more and more popular.

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. 32446-66-5, name is 4,4′-Dicyanobenzophenone, A new synthetic method of this compound is introduced below., Computed Properties of C15H8N2O

123.4 g (388 mmol) 2,2′-Dibromo-biphenyl were dissolved in 450 ml dry THF and cooled to -78 C. 135 ml (323 mmol, 2.5 M in Hexane) n-BuLi was added slowly and the mixture was stirred for 45 min. 4,4′- Dicyanobenzophenone (CAS: 32446-66-5) was dissolved in 400 ml dry THF and cooled to -78 C. The mixture of n-Buli and 2,2′-Dibromo-biphenyl was then transferred to the 4,4′-Dicyanobenzophenonesolution. The reaction was warmed to room temperature over night and after that quenched with water. THF was evaporated in vacuo and the residue was extracted with ethyl acetate and water. The organic phase was dried, filtered and the solvent was removed in vacuo which resulted in 170 g of crude solid. The crude solid was refluxed over night with 2700 ml acetic acid and 200 ml (37%) hydrochloric acid. After cooling to RT the reaction mixture was poured in water and the resulting solid was filtered off, dissolved in (0168) dichloromethane, the solution was washed with water and NaHCO3, the organic phase was dried and the solvent removed in vacuo. The resulting solid was recrystallized in ethyl acetate and finally purified via flash chromatography. The resulting white solid 11 was obtained with a yield of 61 % (88 g , 197 mmol).

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.

Synthetic Route of 251570-03-3, 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 251570-03-3 as follows.

2 -(4-Chloro-3-fluorophenyl)-2-methylpropanenitrileA solution of 4-chloro-3-fluorophenylacetonitrile (1.70 g, 10.0 mmol) in DMF (5 mL) was added dropwise to Sodium hydride (1.00 g, 41.7 mmol) and iodomethane (1.87 mL, 30.0 mmol) in DMF (10 mL) at O0C under a blanket of argon. The resulting slurry was stirred and allowed to warm to ambient temperature for 2 hours. The mixture was concentrated and diluted with ethyl acetate and water and the organic layer washed with further water and the organic layer washed with saturated brine, dried over MgSO4, filtered and evaporated. The crude product was purified by flash silica chromatography, elution gradient 0 to 5% EtOAc in isohexane. Pure fractions were evaporated to dryness to afford 2-(4-chloro-3-(trifluoromethoxy)phenyl)-2-methylpropanenitrile as a yellow oil which solidified on standing.MS (+ve ESI) : Rt = 2.51 min, no mass ion (M+H)+ 1U NMR (400.132 MHz, CDC13) delta 1.71 (6H, s), 7.20 – 7.28 (3H, m), 7.42 (IH, t)

According to the analysis of related databases, 251570-03-3, the application of this compound in the production field has become more and more popular.

Related Products of 874285-03-7, A common heterocyclic compound, 874285-03-7, name is 3-Bromo-2-fluorophenylacetonitrile, molecular formula is C8H5BrFN, 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.

a) 2- (3 -bromo-2-fluorophenyl)ethanamine To a stirred solution of 2-(3-bromo-2-fluoro-phenyl)acetonitrile (10 g, 44.4 mmol, CAS 874285- 03-7) in THF (100 mL) was added borane-tetrahydrofuran complex 1.0 M in THF (88.8 mL, 88.8 mmol) at 0 C. The mixture was stirred at room temperature for 1 hour then heated to reflux overnight. The reaction mixture was then re-cooled to 0 C and MeOH (50 mL) was added. The mixture was heated to reflux for 90 min. The solvent was removed under vacuum and the residue was partitioned between EtOAc and aqueous 1.0 M HC1. The aqueous phase was made basic with aqueous 1.0 M NaOH then extracted with EtOAc. Organic layers were washed with saturated brine, dried (Na2S04) and concentrated in vacuo to afford the title compound (9.1 g, 94%) as a viscous colorless oil which was used in the next step without further purification.

The synthetic route of 874285-03-7 has been constantly updated, and we look forward to future research findings.

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. 69797-49-5, name is 2-Amino-3-methylbenzonitrile, This compound has unique chemical properties. The synthetic route is as follows., Recommanded Product: 2-Amino-3-methylbenzonitrile

Dissolve 2-amino-3-methylbenzonitrile (10.0g, 75.6mmol) and DMSO (7mL) in ethyl acetate (140mL), and dropwise add HBr aqueous solution (3mL) at room temperature for 30-60min. After the dropwise addition is completed, the reaction bottle is closed at 50-80 C, and the reaction time is 1-6h. After the reaction was completed, 1M potassium carbonate aqueous solution (150 mL) was added for washing, and dichloromethane (120 * 3) was used for liquid separation, dried over anhydrous magnesium sulfate, and concentrated under reduced pressure.The target product, 2-amino-5-bromo-3-methylbenzonitrile, was obtained as a yellow solid (13.3 g, 83.1%).

According to the analysis of related databases, 69797-49-5, the application of this compound in the production field has become more and more popular.

Related Products of 191014-55-8, 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. 191014-55-8, name is 4-Fluoro-2-methoxybenzonitrile belongs to nitriles-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

To 4-fluoro-2-methoxybenzonitrile (3.00 g, 20 mmol) and N-iodosuccinimide (NIS) (4.7 g, 21 mmol) under nitrogen was added TFA (35 mL) and the reaction was stirred at room temperature for 20 hours. The volatiles were removed in vacuo and the residue was taken up in 1:1 ethyl acetate:ether and was washed with aqueous sodium bicarbonate and then brine containing enough sodium sulfite to remove the iodine color. The aqueous layers were back extracted with more 1:1 ethyl acetate:ether and the combined organic layers were dried over sodium sulfate and evaporated. The residue was treated with ether/hexanes to afford clean iodo title product as a white solid. 1H-NMR (500 MHz, CDCl3) delta ppm 3.930 (s, 3H), 6.730 (d, J = 9.4 Hz, 1H), 7.900 (d, J = 6.8 Hz, 1H).

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, 4-Fluoro-2-methoxybenzonitrile, other downstream synthetic routes, hurry up and to see.

These common heterocyclic compound, 138642-47-4, name is 2-Bromo-5-methoxybenzonitrile, 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. name: 2-Bromo-5-methoxybenzonitrile

Step A: KOH (4M, 259.66uL, 3.06eq) and Pd(Ph3P)2Cl2 (47.65mg, 67.88umol, 0.20eq) were added to a solutionof the intermediate 12 (200.00mg, 339.42umol, 1.00eq) and 2-bromo-5-methoxyphenyl cyanide (108.00mg, 509.13umol,1.50eq) in 2-methyltetrahydrofuran. The reaction solution was stirred at 65C under nitrogen atmosphere for 13 hours,then cooled to room temperature, and additional Pd(Ph3P)2Cl2 (20.00mg, 33umol, 0.10eq) was added. The reactionsolution was heated to 65C and stirred for another 3 hours to give 87, which was directly used in the next step. Thereaction solution was cooled to room temperature, then methanol (6.00mL) and water (3.00mL) were added and theresulting mixture was stirred at 35C for 2 hours. Lithium hydroxide (15mg) was added, the reaction solution was heatedto 45C and stirred for 3 hours. The reaction solution was cooled to room temperature, adjusted to pH 5 with 2M HCl,diluted with water, extract with ethyl acetate, dried over sodium sulfate, concentrated and purified by silica gel columnchromatography to give the intermediate 88.

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

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. 191014-55-8, name is 4-Fluoro-2-methoxybenzonitrile, This compound has unique chemical properties. The synthetic route is as follows., Recommanded Product: 4-Fluoro-2-methoxybenzonitrile

General procedure: Intermediate 31 (1 S.2S)-2-(4-[(R)-4-(4-Cvano-phenoxy)-7-fluoro-indan-1 -yloxyl-phenyl)- cvclopropanecarboxylic acid ethyl ester (1 S,2S)-2-[4-((R)-7-Fluoro-4-hydroxy-indan-1 -yloxy)-phenyl]-cyclopropanecarboxylic acid ethyl ester (Intermediate 5, 146 mg, 0.41 mmol), 4-fluorobenzonitrile (55 mg, 0.45 mmol), and cesium carbonate (145 mg, 0.45 mmol) are suspended in dry dimethylformamide (1 0 mL) and stirred for 3 hours at 100 C followed by room temperature overnight. The mixture is diluted with water and extracted with ethyl acetate. The organic extract is dried over sodium sulfate, filtered and the solvent removed. The residue is purified by flash chromatography (10% ethyl acetate in cyclohexane) to give the title compound (Yield 62 mg). LC (METHOD 5): tR = 1 .54 min ; Mass spectrum (ES+): m/z = 458 [M+H]+.

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 191014-55-8.