Month: April 2021

Adding a certain compound to certain chemical reactions, such as: 2032-34-0, name is 3,3-Diethoxypropanenitrile, belongs to nitriles-buliding-blocks compound, can increase the reaction rate and produce products with better performance than those obtained under traditional synthetic methods. Here is a downstream synthesis route of the compound 2032-34-0, Computed Properties of C7H13NO2

Charged 3,3-diethoxypropionitrile (20 ml, 19.08 g, 0.1332 mol, 2.25 eq), trifmoroacetic acid (40 ml, 59.56 g, 0.5223 mol, 8.82 eq) and water (10 ml) to the reaction flask at 25-30C under nitrogen atmosphere. Stirred for 6 h at 5-10 C under nitrogen atmosphere. Added dropwise a solution of methyl 2-amino-5-methoxy-4-(3-(4-methyl piperazin-1- yl)propoxy)benzoate in 80 ml ethylacetate within 30-45 min. Stirred the mixture for 10 min. Check the reaction by TLC. Filtered the solid and air dried to afford the title product as light yellow solid. Yield: 19.40 g

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, 3,3-Diethoxypropanenitrile, other downstream synthetic routes, hurry up and to see.

Reference of 3939-09-1, 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. 3939-09-1, name is 2,4-Difluorobenzonitrile belongs to nitriles-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

Benzyl alcohol (0.77 g, 7.2 mmol) was added to a stirred suspension of potassium tert-butoxide (0.97 g, 8.6 mg) in dioxane (15 ml) at room temperature. After 10 minutes of stirring at room temperature 2,4-difiuorobenzonitrile (1.00 g, 7.2 mmol) was added in one portion. After another 90 minutes water (10 ml) was added and the mixture extracted with diethyl ether (3×10 ml), the combined organic phases were dried using a phase separator and concentrated to solids. The crude material was purified by column (0491) chromatography using silicon dioxide gel, eluting with 25-50% dichloromethane in petroleum ether to afford 2-(benzyloxy)-4-fluorobenzonitrile as a white solid (1.33 g, 81%). (0492) [00317] A cold solution of borane (1.4 ml, 1 M in tetrahydrofuran) was added to 2- (benzyloxy)-4-fluorobenzonitrile (208 mg, 915 mutauetaomicron). After 15 hours of stirring at room temperature additional borane (1.4 ml, 1 M in tetrahydrofuran) was added. After another 19 hours of stirring additional borane (1.0 ml, 1 M in tetrahydrofuran) was added. After 3 hours the mixture was added to sodium hydroxide (5 ml, 1 M aqueous), extracted with ethyl acetate (3×5 ml), the combined organic phases were dried using a phase separator and concentrated afford [2-(benzyloxy)-4-fluorophenyl]methanamine as oil (260 mg, quantitative). This material was used without further purification. (0493) [00318] N-Methyl-4-piperidone (150 mg, 1.32 mmol) was added to a stirred solution of [2-(benzyloxy)-4-fluorophenyl]methanamine (204 mg, 882 mueta omicron) in ethanol (5 ml), after 5 minutes sodium triacetoxyborohydride (372 mg, 1.76 mmol) was added. After 6 hours the reaction mixture was concentrated, redissolved in dichloromethane (5 ml), washed with sodium hydroxide (5 ml, 1 M aqueous), the aqueous phase was extracted with additional dichloromethane (2×1 ml), the combined organic phases were dried using a phase separator, and concentrated to afford the desired intermediate as a yellow oil (253 mg, 87 %).

The synthetic route of 2,4-Difluorobenzonitrile has been constantly updated, and we look forward to future research findings.

Electric Literature of 6629-04-5, 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. 6629-04-5 name is N-Cyanoacetylurethane, 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.

To a solution of B (25 g, 160 mmol), propionaldehyde (9.3 g, 160 mmol) and Sg (5.1 g, 160 mmol) in DMF (30 mL) at 0C under nitrogen was added morpholine (7.9 g, 90 mmol). Reaction mixture was heated at 50C for 30 min, monitored by TLC. Solvent was removed in vacuo, and the mixture poured into ice water (50ml), extracted with EtOAc, washed with water and brine and concentrated. Crude material was purified by column chromatography (silica gel, EtOAc:PE = 1 : 1) to give 5 (6.8g, 18%) as a yellow solid.

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

Electric Literature of 120315-65-3, These common heterocyclic compound, 120315-65-3, name is 4-Bromo-3-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.

A mixture of 4-bromo-3-methoxybenzonitrile(lg, 4.72 mmol), 4,4,4′,4′,5,5,5′,5′- octamethyl-2,2′-bi(l,3,2-dioxaborolane) (1.796 g, 7.07 mmol), K3P04 (1.157 g, 11.79 mmol) and PdCl2(dppf) CH2C12 adduct (0.207 g, 0.283 mmol) in dioxane (12 mL) was degassed and then heated at 90 C for 3 h. The reaction was cooled to rt and was filtered through a pad of CELITE. The solvent was removed. Normal phase chromatography afforded X-lb as brown oil (1.7 g, 5.76 mmol, 100%). LC-MS (ESI) of the boronic acid m/z: 178.0 [M+H]+.

Statistics shows that 4-Bromo-3-methoxybenzonitrile is playing an increasingly important role. we look forward to future research findings about 120315-65-3.

Synthetic Route of 64248-64-2, The chemical industry reduces the impact on the environment during synthesis 64248-64-2, name is 2,5-Difluorobenzonitrile, I believe this compound will play a more active role in future production and life.

Step A: 5-Fluoro-2-hydroxybenzonitrile (23t): 2,5-Difluorobenzonitrile (14.9 g, 107 mmol) and benzyl alcohol (11.1 mL, 11.6 g, 107 mmol) were dissolved in DMF (330 mL) and cooled to 0 C. Sodium hydride (60% in oil, 6.40 g, 161 mmol) was added to the solution at 0 C. and the reaction mixture was allowed to warm to room temperature. After stirring for 1 hour at room temperature, the reaction solution was cooled to 0 C. and water (330 mL) was gradually added to the solution. The mixture was transferred to a separatory funnel and extracted three times with 500 mL of Et2O. The combined organic layer was washed twice with 100 mL of water, brine once, then dried over MgSO4. After filtration, the solution was concentrated under reduced pressure to obtain a crude pale yellow solid. The crude solid was dissolved in MeOH (500 mL). To the solution was added 10% palladium on activated carbon under a nitrogen atmosphere. Replacing nitrogen gas with hydrogen gas, reaction mixture was stirred at room temperature (if the reaction did not proceed in 30 minutes, the Pd/C was filtered off and the reaction was set up again). After 2 hours of stirring, the palladium on carbon was filtrated off and washed with MeOH. The solution was concentrated under reduced pressure to obtain a pale yellow solid. The solid was recrystallized from hot toluene (100 mL) by addition of hexane (10 mL) followed by cooling to 0 C. The obtained white needles were washed with 1:1 mixture of toluene and hexane (7.23 g, 49% yield). Mother liquor was concentrated and purified on silica gel with Et2O/hexane (2:3-1:1) to afford the desired compound (23t) (6.94 g, 47% yield). Total 14.2 g (96% yield) over 2 steps. 1H-NMR (400 MHz, d6-DMSO) delta 11.09 (s, 1H), 7.58 (dd, J=8.4, 3.2 Hz, 1H), 7.40 (td, J=8.6, 3.2 Hz, 1H), 7.03 (dd, J=9.2,4.4 Hz, 1H) ppm.

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, 2,5-Difluorobenzonitrile, other downstream synthetic routes, hurry up and to see.

Adding a certain compound to certain chemical reactions, such as: 50670-64-9, name is 5-Amino-2-methylbenzonitrile, belongs to nitriles-buliding-blocks compound, can increase the reaction rate and produce products with better performance than those obtained under traditional synthetic methods. Here is a downstream synthesis route of the compound 50670-64-9, Formula: C8H8N2

To a stirred solution of 5-Amino-2-methylbenzonitrile (4.00 g, 30.27 mmol) in 33% sulfuric acid (45 mL) was added a solution of sodium nitrite (2.09 g, 30.27 mmol) in water (15 mL) at 5C. The temperature was kept below 5C. In a separated flask, concentrated sulfuric acid (30 mL) was added cautiously to a stirred solution of sodium sulfate (21.50 g, 151.33 mmol) in water (15 mL). The slurry was heated to reflux. The prepared diazonium salt was added dropwise to the refluxing mixture and the reflux was continued for 2 hours. The mixture was cooled slowly to room temperature. The mixture was extracted with ethyl acetate (2 x 100 mL) and the combined extracts were washed with water (2 x 150 mL). The organic layer was extracted with aqueous 10% NaOH solution (2 x 100 mL). The alkaline extract was acidified with cone. HC1 and extracted with EtOAc (2 x 100 mL). The combined organic layers were dried over MgSCL, filtered and the solvent was evaporated in vacuo to afford the title compound as a red solid and pure enough to be used as such (2400 mg, 60% yield). 1H NMR (300MHz, CHCL-d) 9.46 (bs, 1H), 7.16 (d, / = 8.4 Hz, 1H), 7.06 (d, / = 2.7 Hz, 1H), 6.97 (dd, / = 8.4 and 2.7 Hz, 1H ), 2.45 (s, 3H).

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-Amino-2-methylbenzonitrile, other downstream synthetic routes, hurry up and to see.

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. 263159-64-4, name is 2-Bromo-3-methylbenzonitrile, A new synthetic method of this compound is introduced below., SDS of cas: 263159-64-4

Step 3: A mixture of compound 249 (1 1 g, 56.1 mmol), NBS (10 g, 56.1 mmol) and BPO (81 mg, 0.34 mmol) in CCI4 (150 mL) was heated at reflux overnight. TLC (petroleum ether / EtOAc = 5:1 ) showed the reaction was completed. The mixture was filtered and the filtrate was concentrated. The residue was purified by column chromatography over silica gel (petroleum ether / EtOAc = 20:1 ) to yield compound 250 (9.6 g, 62%) as a white solid. 1H NMR (400 MHz, CDCI3) delta 7.69- 7.67 (d, 1 H), 7.63-7.61 (d, 1 H), 7.45-7.41 (t, 1 H), 4.61 (s, 2H)

The synthetic route of 263159-64-4 has been constantly updated, and we look forward to future research findings.

Reference of 70591-86-5, 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. 70591-86-5 name is 3-Bromobenzoylacetonitrile, 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.

A mixture of 3-(3-bromophenyl)-3-oxopropanenitrile (35 g, 156 mmol) and hydrazine hydrate (11.34 mL, 234 mmol) in ethanol (600 mL) was refluxed for 16 h. Mixture was then cooled and concentrated in vacuuo. Crude product was diluted with dichloromethane and stirred for 5 min. Solids were filtered and dried to afford 3-(3-bromophenyl)-1H-pyrazol-5-amine (30 g, 126 mmol, 81 % yield) as off-white solid. 1H NMR (400 MHz, DMSO-d6) delta 12.02 (br. s., 0.4H), 11.66 (br. s., 0.6H), 7.86 (t, J=1.6 Hz, 1H), 7.67 (d, J=7.5 Hz, 1H), 7.45 (d, J=6.8 Hz, 1H), 7.37 – 7.18 (m, 1H), 5.78 (br. s., 1H), 5.08 (br. s., 1.2H), 4.68 (br. s., 0.8H). LCMS (M+H) = 240.1.

At the same time, in my other blogs, there are other synthetic methods of this type of compound, 3-Bromobenzoylacetonitrile, and friends who are interested can also refer to it.

Electric Literature of 4426-11-3, 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. 4426-11-3, name is Cyclobutanecarbonitrile belongs to nitriles-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

Example 240A 1-[2-(trifluoromethyl)pyridin-4-yl]cyclobutanecarbonitrile A solution of cyclobutanecarbonitrile (1.36 g, 16.77 mmol) and 4-chloro-2-(trifluoromethyl)pyridine (2.89 g, 15.92 mmol) in anhydrous THF (55 mL) was chilled to -75 C. 1.0M lithium hexamethyl disilazide (24 mL, 24.00 mmol) in THF was added dropwise, and the reaction was permitted to warm to ambient temperature overnight. The reaction was quenched with saturated NH4Cl solution (200 mL) and extracted with EtOAc (300 mL). The organic layer was washed with saturated NH4Cl solution (200 mL), dried over Na2SO4, filtered, and concentrated. The residue was chromatographed on silica (5-50% EtOAc in heptane) to give Example 240A (2.162 g, 7.65 mmol, 48% yield) as an orange oil. LC/MS (APCI+): m/z 227 (M+H). 1H NMR (300 MHz, DMSO-d6) delta 8.84 (d, J=5.1 Hz, 1H), 8.00 (d, J=1.3 Hz, 1H), 7.90-7.82 (m, 1H), 2.89-2.66 (m, 4H), 2.42-2.22 (m, 1H), 2.13-1.90 (m, 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, Cyclobutanecarbonitrile, other downstream synthetic routes, hurry up and to see.

Reference of 261951-81-9, 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. 261951-81-9, name is 3-Fluoro-2-(trifluoromethyl)benzonitrile belongs to nitriles-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

A solution of 3-fluoro-2- (trifluoromethyl)benzonitrile g, 6.3 mmol) and piperazine (0.72 g, 8,4 mmol) in acetonitrile (6 ml) was heated under microwave radiation at 150 C for 15 minutes. The reaction mixture was poured into water (50 ml) and the aqueous phase was extracted with ethylacetate (3×50 ml). The combined organic phases was dried (MgS04), filtered and evaporated to dryness. Purification by flash column chromatography (ethylacetate/methanol, 1:1) gave the title compound: 1.1 g. MS m/z (rel. intensity, 70 eV) 255 (M+, 16), 214 (11), 213 (bp), 171 (8), 151 (7).

The synthetic route of 3-Fluoro-2-(trifluoromethyl)benzonitrile has been constantly updated, and we look forward to future research findings.