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 49744-93-6 as follows. Product Details of 49744-93-6

Step 3 Ethyl 3-(4-cyanophenyl)-3-oxopropanoate (64 mg, 0.3 mmol) in THF (1 ml) and DMFDMA (0.3 mmol) was heated at 70 C. for 3 hours. The solution was added to a mixture of the guanidine from Step 2 (123 mg, 0.3 mmol), 1.0 M sodium ethoxide in ethanol (0.35 ml) and ethanol (1 ml). The mixture was then heated overnight at 80 C., cooled, diluted with dichloromethane, then washed with saturated sodium bicarbonate solution. The organic layer was concentrated in vacuo, redissolved in acetonitrile and the product precipitated with water. HPLC: 27.63 min (85% pure) MS: MH+=448 C22H21N7O4=447 g/mol

According to the analysis of related databases, 49744-93-6, the application of this compound in the production field has become more and more popular.

Synthetic Route of 133541-45-4, A common heterocyclic compound, 133541-45-4, name is 4-Bromo-2,5-difluorobenzonitrile, molecular formula is C7H2BrF2N, 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 suspension of sodium hydride (4.04 g, 100 mmol, 60 % purity) in THF (25 mL) was added tert-butyl N-(2-hydroxypropyl)carbamate (8.84 g, 50.5 mmol) at 0 “C. The resulting mixture was stirred at 0 C for 0.5 h, then a solution of 4-bro mo-2,5-difluorobenzonitrile (10 g, 45.9 mmol) in THF (25 mL) was added. The mixture was stirred at 0 C for 0.5 h. The reaction mixture was diluted with water and extracted with ethyl acetate. The combined organic layers were washed with brine, dried over sodium sulfate, filtered and concentrated under reduced pressure to give a residue, which was purified by column chromatography (silica gel, petroleum ether/ethyl acetate = 50/1 to 10/1 ) to give the desired product (13 g, 34.8 mmol, 76% yleld) as a white solid.MS (M+H+): 397.11H NMR (400 MHz, CDCI3) delta [ppm]: 7.33-7.30 (t, J = 6Hz, 1 H), 7.27-7.24 (t, J = 6Hz, 1 H), 4.99 (s, 1 H), 4.57 (s, 1 H), 3.53-3.48 (m, 1 H), 3.33-3.28 (m, 1 H), 1 .62-1 .45 (q, 9H), 1.36-1.26 (m, 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 of 32446-66-5, 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. 32446-66-5, name is 4,4′-Dicyanobenzophenone, This compound has unique chemical properties. The synthetic route is as follows.

EXAMPLE 3 4-[alpha-(4-Cyanophenyl)-alpha-hydroxy-5-thiazolylmethyl]-benzonitrile Analogously to Example 1, the title compound is prepared starting from 0.512 ml of diisopropylamine, 2.44 ml of a 1.6M n-butyllithium solution, 530 mg of 2trimethylsilylthiazole and 603 mg of 4,4′-dicyanobenzophenone in THF at -70 and with working up in the same manner. Purification of column chromatography (SiO2, hexane/ethyl acetate 2:2) yields the title compound in pure for. TLC (hexane/ethyl acetate 2:2) Rf =0.2; 1 H-NMR (CDCl3): delta(ppm)=4.39 (s,1H), 7.42 (d,1H), 7.54 and 7.7 (m,8H), 7.88 (d,1H).

The chemical industry reduces the impact on the environment during synthesis 4,4′-Dicyanobenzophenone. I believe this compound will play a more active role in future production and life.

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.

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.

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.

Application of 57381-39-2, 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 57381-39-2 as follows.

EXAMPLE 6 4,2′-Difluoro-5′-(5-methyl-4-oxo-4,5-dihydroimidazo[4,5-c]pyridin-1-yl)biphenyl-2-carbonitrile 2-Bromo-5-fluorobenzonitrile was converted to 5-fluoro-2-(4,4,5,5-tetramethyl-[1,3,2]dioxaborolan-2-yl)benzonitrile as described in Example 2 to give a straw-coloured solid: deltaH (360 MHz, CDCl3) 1.38 (12H, s), 7.27 (1H, ddd, J 8, 8 and 2), 7.39 (1H, dd, J 9 and 2), 7.90 (1H, dd, J 8 and 6). 1-(3-Bromo-4-fluorophenyl)-5-methyl-1,5-dihydroimidazo[4,5-c]pyridin-4-one was coupled to 5-fluoro-2-(4,4,5,5-tetramethyl-[1,3,2]dioxaborolan-2-yl)benzonitrile, in the same way as in Example 1, to give 4,2′-difluoro-5′-(5-methyl-4-oxo-4,5-dihydroimidazo[4,5-c]pyridin-1-yl)biphenyl-2-carbonitrile as an off-white solid (360 mg, 55%): deltaH (400 MHz, d6-DMSO) 3.54 (3H, s), 6.67 (1H, d, J 7), 7.61 (1H, d, J 7), 7.69 (1H, t, J 9), 7.75-7.87 (4H, m), 8.09 (1H, dd, J 9 and 3), 8.38 (1H, s); m/z (ES+) 363 [MH+].

According to the analysis of related databases, 57381-39-2, the application of this compound in the production field has become more and more popular.

Application of 1105665-42-6, These common heterocyclic compound, 1105665-42-6, name is 5-Bromo-2,3-difluorobenzonitrile, 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.

2,3-difluoro-5-(4,4,5,5-tetramethyl-1,3,2-dioxaborolan-2-yl)benzonitrile (0275) To a solution of 5-bromo-2,3-difluorobenzonitrile (140 mg, 0.64 mmol) in 1,4-dioxane (7 mL) were added 4,4,5,5-tetramethyl-2-(tetramethyl-1,3,2-dioxaborolan-2-yl)-1,3,2-dioxaborolane (179.4 mg, 0.71 mmol), Pd(dppf)Cl2 (26.2 mg, 0.04 mmol) and potassium acetate (126 mg, 1.28 mmol) at room temperature. The resulting mixture was stirred for 2 h at 120 C. and then water (10 mL) was added. The mixture was extracted with ethyl acetate (30 mL×3). The organic phases were combined, washed with brine and dried over sodium sulfate. The solvent was removed under reduced pressure to yield 2,3-difluoro-5-(tetramethyl-1,3,2-dioxaborolan-2-yl)benzonitrile as brown oil (200 mg, crude). MS: m/z=266.0 [M+H]+.

The synthetic route of 1105665-42-6 has been constantly updated, and we look forward to future research findings.

Electric Literature of 220239-65-6,Some common heterocyclic compound, 220239-65-6, name is 4-fluoro-3-(trifluoromethyl)phenylacetonitrile, molecular formula is C9H5F4N, 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.

EXAMPLE H1 Preparation of 2-(4-fluoro-3-trifluoromethyl-phenyl)-ethylamine hydrochloride A solution of (4-fluoro-3-trifluoromethyl-phenyl)-acetonitrile (4.00 g, 19.3 mmol) in THF was added dropwise at 0-5 C. to a suspension of lithium aluminum hydride (1.61 g, 42.4 mmol) in diethyl ether (20 mL). The ice bath was removed and the reaction mixture was allowed to reach RT, then heated at reflux overnight. After cooling to 0 C., saturated aq. sodium sulfate solution was carefully added. After the initial exothermic reaction had subsided, the flask was allowed to warm to ambient temperature and solid magnesium sulfate (dry) was added to dry the suspension, which was subsequently filtered and washed with diethyl ether. After removal of the solvent, the residue was dissolved in diethyl ether (50 mL), treated with hydrogen chloride solution (2.6 M in diethyl ether, 8 mL), and evaporated to dryness, leading to a solid orange foam. This residue was dissolved in dichloromethane (200 mL), and treated with water (100 mL), followed by 1 M aq. hydrochloric acid solution (50 mL), and stirred for 15 minutes, then the organic layer was separated and extracted a second time with 1 M aq. hydrochloric acid solution (50 mL). The combined aqueous phases were then washed with dichloromethane (50 mL), treated with concentrated aq. sodium hydroxide solution to adjust the pH to 12, and extracted twice with dichloromethane. The combined organic phases were washed with water and dried over magnesium sulfate. After filtration and evaporation of the solvent, the residue was dissolved in diethyl ether (5 mL), treated with hydrogen chloride solution (2.6 M in diethyl ether, 2 mL), and stirred for 10 min. The precipitate was collected by filtration and dried to afford the title compound (632 mg, 13%). White solid, MS (ISP) 208.2 (M-Cl)+.

The synthetic route of 220239-65-6 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. 425379-16-4, name is 2-Bromo-3-fluorobenzonitrile, This compound has unique chemical properties. The synthetic route is as follows., COA of Formula: C7H3BrFN

(4aS,5S)-1-(4-Fluorophenyl)-4a-methyl-5-[2-(4,4,5,5-tetramethyl-1,3,2-dioxaborolan-2-yl)ethyl]-1,4,4a,5,6,7-hexahydrocyclopenta[f]indazol-5-ol (13) (200 mg, 0.456 mmol), 2-bromo-3-fluorobenzonitrile (91 mg, 0.456 mmol), 1,1′-bis(di-tert-butylphosphino)ferrocene palladium dichloride (30 mg, 0.046 mmol), and Cs2CO3 (446 mg, 1.37 mmol) in degassed toluene(0.9 mL)/water (0.3 mL) were heated at 80 C for 1 h. The reaction was quenched with water and extracted with EtOAc (×3). The combined organic extracts were dried over MgSO4, filtered, and concentrated in vacuo. The residue was purified by flash chromatography on Silica, eluting with a gradient of 0-100% EtOAc in hexanes to afford 14 (139 mg, 71%) as a white solid; 1H NMR (CDCl3, 500 MHz): delta 7.50 (s, 1H), 7.44-7.40 (m, 3H), 7.33-7.25 (m, 2H), 7.17 (t, J = 8.3 Hz, 2H), 6.15 (s, 1H), 3.18 (td, J = 12.7, 4.5 Hz, 1H), 2.97 (td, J = 12.6, 4.8 Hz, 1H), 2.84 (d, J = 15.4 Hz, 1H), 2.65 (dd, J = 19.0, 9.8 Hz, 1H), 2.53-2.42 (m, 2H), 2.34-2.26 (m, 1H), 2.07-1.98 (m, 1H), 1.88-1.80 (m, 1H), 1.75-1.67 (m, 1H), 1.17 (s, 3H), 0.90-0.82 (m, 1H); MS (ESI): m/z = 432.09 (MH+), 100% pure by LC-MS.

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 425379-16-4.