Tag: M.W=100-200

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. 459-22-3, name is 4-Fluorophenylacetonitrile, A new synthetic method of this compound is introduced below., Recommanded Product: 4-Fluorophenylacetonitrile

Reagents and conditions: (a) EtONa, EtOH, refluxing; (b) CH3NHNH2, HC1, EtOH,MW, 100C, 40 mm; (c) Fmoc-(R)-3-amino-4-(4-fluorophenyl)butanoyl chloride,DCM, then DBU. A mixture of 1.8 ml (15 mmol) of ethyl 2,2,2-trifluoroacetate (ib)and 0.96 g (7.1 mmol) of 2-(4-chloro-2-fluorophenyl)acetonitrile (3a) in 10 ml ofethanol was slowly dropped into hot solution of 1.2 g of sodium in 20 ml of ethanol.The mixture was refluxed overnight. The solution turns red. After cooled down, thesolution was poured into 250 ml of cold water acidified with 10 ml concentrated HC1.The mixture was extracted with ethyl acetate. The ethyl acetate extraction was washedwith water, brine and dried over Mg504. Ethyl acetate was removed and the residualreddish oil of 4,4,4-trifluoro-2-(4-fluorophenyl)-3 -oxobutanenitrile (3c) was obtained in1.3 g. The raw material was dissolved in 10 ml of ethanol and used in next step withoutfurther purification. A mixture of 2.8 ml of the above ethanol solution and 125pi ofmethylhydrazine with 0.2 ml of concentrated HC1 was irradiated in microwave oven at100C for 40 mm. The solution was treated with saturated NaHCO3 and extracted byethyl acetate. The organic layer was washed with water, brine, dried over Mg504 andconcentrated. The yellow residue was subjected to flash chromatography purificationwith MeOHIDCM to give 165 mg of 3-(trifluoromethyl)-4-(4-fluorophenyl)-1-methyl-1H-pyrazol-5-amine (3d) as light yellow solid. ?H NMR (500 MHz, CDC13) 7.32 (s,2H), 7.14 (t, J = 8.0 Hz, 2H), 3.76 (d, J = 33.5 Hz, 3H), 3.65 (s, 2H). M/Z =260.6(M+1). To a solution of Fmoc-(R)-3-amino-4-(4-fluorophenyl)butanoyl chloride (43mg, 0.20 mmol) produced from Fmoc-(R)-3-amino-4-(4-fluorophenyl)butanoic acid(from Chem Impex International) and thionyl chloride in 10 ml of anhydrous DCM were slowly added 3 -(trifluoromethyl)-4-(4-fluorophenyl)- 1-methyl-i H-pyrazol-5 – amine obtained as described above (39 mg, 0.15 mmol) in 5 ml of anhydrous DCM. The reaction mixture was stirred at room temperature overnight. The reaction mixture was quenched with methanol and solvents were removed. The residue was purified via silicagel with MeOHIDCM to obtained Fmoc protected product. Fmoc protected product was dissolved in 10 ml of ethyl acetate and 0.15 mmol of DBU was added. After 20mm 20 ml of ethyl acetate was added and mixture was washed with 20 ml of water. The organic layer was collected and solvent was removed. The residue was dissolved in MeOH and acidified with 0.2N HC1. The solution was purified via preparatory RP-HPLC, elutingwith H20/CH3CN gradient (+0.05% TFA). Product fractions are collected and concentrated. The residue is dissolved in a small amount of 2M HC1 in methanol and, after concentration in vacuo, 50 mg of Compound (3) is obtained as an HC1 salt. ?H NIVIR (500 IVIFIz, MeOD) 7.40 – 7.08 (m, 6H), 7.02 (t, J = 8.8 Hz, 2H), 3.77 (d, J = 15.4 Hz, 3H), 3.37 (dt, J = 7.9, 6.6 Hz, 1H), 2.64 (m, 2H), 2.42 (m, 2H). M/Z 439.4(M+i).

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.

Related Products of 191014-55-8, The chemical industry reduces the impact on the environment during synthesis 191014-55-8, name is 4-Fluoro-2-methoxybenzonitrile, I believe this compound will play a more active role in future production and life.

General procedure: To a solution of (4S,5S)-4-hydroxy-5-methylpyrrolidin-2-one 7 33 (7.00 g, 60.8 mmol) in THF (120 mL) was added sodium bis(2-methoxyethoxy)aluminium dihydride (70% in toluene, 59.7 mL, 215 mmol) slowly at 5 C. After stirring at 70 C for 3 h, the reaction mixture was cooled to 5 C followed by addition of sodium carbonate decahydrate (26.1 g, 91.2 mmol). The mixture was stirred at room temperature for 16 h, diluted with THF, and the precipitate was filtered off. The filtrate was concentrated in vacuo, and the residue was dissolved in DMSO (80 mL). To the solution was added lithium carbonate (8.99 g, 122 mmol) and 2-chloro-4-fluorobenzonitrile (9.46 g, 60.9 mmol), and the mixture was stirred at 100 C for 1 h. The mixture was diluted with EtOAc and H2O, and the organic layer was dried over anhydrous MgSO4 and concentrated in vacuo. The residue was purified by silica gel column chromatography (hexane-EtOAc) to give 10 (10.7 g, 74%) as a colorless solid. 1H NMR (300 MHz, CDCl3) delta: 1.18 (3H, d, J = 6.6 Hz), 1.82 (1H, d, J = 5.5 Hz), 2.01-2.14 (1H, m), 2.25-2.35 (1H, m), 3.19-3.28 (1H, m), 3.43-3.51 (1H, m), 3.89-3.98 (1H, m), 4.43-4.52 (1H, m), 6.43 (1H, dd, J = 8.9 and 2.4 Hz), 6.56 (1H, d, J = 2.4 Hz), 7.42 (1H, d, J = 8.9 Hz). MS (ESI) m/z 237 [(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, 4-Fluoro-2-methoxybenzonitrile, other downstream synthetic routes, hurry up and to see.

1349718-98-4, name is 2,4-Dichloro-6-fluorobenzonitrile, belongs to nitriles-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. SDS of cas: 1349718-98-4

To a solution of 2,4-dichloro-6-fluorobenzonitrile (3.87 mmol) in 15 mL THF was added a solution of BH3 (15.5 mmol, 1M in THF) and the mixture was stirred at 60 C. for 1 h. After cooling to 0 C., water was added followed by MeOH and the mixture was then heated to 70 C. for 10 min. The solvent was evaporated, the residue was taken up in water and EtOAc. The aqueous phase was separated, basified with 1M NaOH and it was extracted 3 times with EtOAc. The combined organic layers were dried over MgSO4 and concentrated in vacuo to obtain the desired product as yellow oil. LC-MS (A): tR=0.39 min; [M+CH3CN+H]+: 234.90.

The synthetic route of 1349718-98-4 has been constantly updated, and we look forward to future research findings.

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. 175596-01-7, name is Methyl 4-cyano-2-fluorobenzoate, A new synthetic method of this compound is introduced below., COA of Formula: C9H6FNO2

Step 2: methyl 4-[amino(hydroxyimino)methyl]-2-fluorobenzoate To a solution of methyl 4-cyano-2-fluorobenzoate, obtained in Step 1 (486.8 mg; 2.72 mmol) in abs. EtOH (6 ml_) was added hydroxylamine (0.8 ml 13.6 mmol; 5 eq.) (50% in water) and the mixture was heated at 74C overnight. After cooling, a product precipitated. The precipitate was filtered off and dried under vacuum to afford Intermediate 1 as an off-white solid (267.10 mg; 46%). 1H-NMR (DMSO-d6, 300MHz) delta 10.09 (s, 1 H), 7.92 (t, J = 7.91 Hz, 1 H), 7.69 (dd, J = 1.70 Hz, J = 8.10 Hz, 1 H), 7.64 (dd, J = 1.51 , J = 12.81 , 1 H), 6.05 (s, 2H), 3.90 (s, 3H). HPLC (Method B) Rt 2.99 min (Purity: 100%).

The synthetic route of 175596-01-7 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. 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.

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.

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.

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.

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.

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.