Month: May 2021

Adding a certain compound to certain chemical reactions, such as: 1009-35-4, name is 4-Fluoro-3-nitrobenzonitrile, 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 1009-35-4, HPLC of Formula: C7H3FN2O2

The intermediate E lot used in this Example existed as ~3: 1 S:R mixture of phenyl chirality. To a vial charged with (S)-3-((lr,4S)-4-aminocyclohexyl)-5,5- dimethyl-4-phenyloxazolidin-2-one (0.150 g, 0.520 mmol) were added ACN (1.734 mL), TEA (0.145 mL, 1.040 mmol) and 4-fluoro-3-nitrobenzonitrile (commercially available from Alfa Aesar, Ward Hill, MA) (0.086 g, 0.520 mmol) respectively. The resulting orange solution was shaken at 80°C overnight. The resulting mixture was dried under reduced pressure and the material thus obtained was purified with a 25 g SNAP column ramping EtOAc in heptane from 0 – 100percent with 10percent DCM throughout providing 4-(((l S,4r)-4-((S)-5,5-dimethyl-2-oxo-4-phenyloxazolidin-3- yl)cyclohexyl)amino)-3-nitrobenzonitrile (0.172 g, 0.396 mmol, 76 percent yield) as a yellow solid. H NMR (400 MHz, CDC13) delta = 8.47 (d, J= 2.0 Hz, 1 H), 8.25 (d, J= 7.4 Hz, 1 H), 7.58 – 7.51 (m, 1 H), 7.47 – 7.28 (m, 4 H), 7.14 (br. s., 1 H), 6.85 (d, J = 9.2 Hz, 1 H), 4.39 (s, 1 H), 3.50 – 3.33 (m, 2 H), 2.24 – 2.06 (m, 3 H), 2.02 – 1.93 (m, 1 H), 1.90 – 1.79 (m, 1 H), 1.62 – 1.49 (m, 4 H), 1.47 – 1.26 (m, 2 H), 0.92 (s, 3 H). m/z (ESI) 435.2 (M+H)+.

At the same time, in my other blogs, there are other synthetic methods of this type of compound, 4-Fluoro-3-nitrobenzonitrile, and friends who are interested can also refer to it.

Electric Literature of 89001-53-6, 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. 89001-53-6 name is 2-Methyl-4-nitrobenzonitrile, 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.

Example 1; Preparation of Compound 6c6c; Step A: Preparation5,6-Dihydro-5-oxo-9-nitro-indeno[l,2-c]isoquinolineTo arefluxing mixture of 2-methyl-4-nitro-benzonitrile (32.4 g, 0.2 mol) and NBS (44.470 g, 0.25 mol) in CCl4 (300 ml) was added ATON (0.325 g) and the resultant EPO reaction mixture was refluxed for 4 hours. The reaction mixture was treated with ABBN (0.325 g, 31 mmol) and refluxed further for 4 hours. The reaction mixture was filtered, and the filtered succinimide was washed with CCl4. The filtrate was concentrated in vacuo to provide a bromo compound (46 g). The bromo compound was dissolved in MeCN (200 ml), and to the reaction mixture was added homophthalic anhydride (30.780 g, 0.19 mol) at room temperature and under inert atmosphere. The reaction mixture was then treated with a solution of triethylamine (84 ml, 0.6 mol) in acetonitrile (100 ml). The reaction mixture was refluxed for 8 hours. The precipitate that formed was removed by filtration and washed with MeCN (100 ml). The washed precipitate was suspended in DMF (300 ml), which was heated at 130 0C, then cooled and filtered. The resultant solid was washed with DMF (100 ml) and dried under vacuum to provide 5,6-Dihydro-5-oxo- 9-nitro-indeno[l,2-c]isoquinoline as a pale yellow solid (18.310 g, 33%). 1H-NMR (DMSO-d6): delta, 4.09 (s, 2H), 7.56 (m, IH), 7.81 – 7.82 (m, 2H), 8.17 (d, J = 8.4 Hz, IH), 8.26 – 8.34 (m, 2H), 8.44 (s, IH), 12.47 (s, IH).

At the same time, in my other blogs, there are other synthetic methods of this type of compound, 2-Methyl-4-nitrobenzonitrile, and friends who are interested can also refer to it.

Electric Literature of 21524-39-0, 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. 21524-39-0, name is 2,3-Difluorobenzonitrile belongs to nitriles-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

A mixture of 2, 3-difluorobenzonitrile (19. 0 g, 137 mmol) and ethanol (200 ml) pre-saturated with ammonia gas was heated at 140C in an autoclave for 8 h (terminal pressure 200 psi). The mixture was allowed to cool to ambient temperature and evaporated to dryness. The residue was dissolved in water (400 ml) and extracted with diethyl ether (2 x 300 ml). The combined organics were washed with water (300 ml) and brine (250 ml), dried over anhydrous magnesium sulfate, filtered and evaporated. Trituration with isohexane (150 ml) afforded 2-amino-3-fluorobenzonitrile (9.8 g, 50%) as an off-white solid: 1H NMR (360 MHz, CDCl3) 8 4.47 (2H, s), 6.65-6. 71 (1H, m), 7.14-7. 20 (2H, m).

The synthetic route of 2,3-Difluorobenzonitrile 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. 16532-79-9, name is 4-Bromophenylacetonitrile, This compound has unique chemical properties. The synthetic route is as follows., Product Details of 16532-79-9

EXAMPLE 3; Synthesis of N2-((lS)-l-{4′-[1-(aminocarbonyl) cyclopropyl] biphenyl-4-yl}-2, 2-difluoroethyl)-Nl-(l- cyanocyclopropyl)-4-fluoro-L-leucinamide; F F F N ion Razz H,, N Nez H2N Step 1 : Preparation of 1-(4-bromophenyl) cyclopropanecarbonitile; To a room temperature solution of 4-bromophenylacetonitrile (18.0 g) in a solution of 22 mL of sodium hydroxide (50% in water W/W) were added 1-bromo-2-chloroethane and (12.0 mL) and benzyltriethylammonium chloride (627 mg). The mixture was heated at 60 C overnight. The reaction mixture was cooled to room temperature and diethyl ether was added (300 mL) and partitioned. The ether layer was washed with water (100 mL), hydrogen chloride (100 mL, 10% HCI in water) and brine. Then dried with magnesium sulfate and the solvent removed in vacuo. The residue was purified by swish using diethyl ether and hexanes to yield the title compound. ‘H NMR (CD3COCD3) 8 7.60 (2H, d), 7.35 (2H, d), 1.74-1. 80 (2H, m), 1.52-1. 57 (2H, m).

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 16532-79-9.

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. 67832-11-5, name is 4-Bromo-2-methylbenzonitrile, A new synthetic method of this compound is introduced below., Quality Control of 4-Bromo-2-methylbenzonitrile

Preparation 13A; 2-methyl-4-? H-pyrrolor2.3-b1Pyridi?-1 -vObenzonitrile; A mixture of 4-bromo-2-methylbenzonitrile (5.45 g, 27.8 mmol), N, N’- dimethyiethyienediamine (0.6 mL, 5.56 mmol), CuI (530 mg, 2.78 mmol), and sodium iodide (7.9 g, 52.8 mmol) in toluene (50 mL) was heated at reflux for 28h. K3PO4 (12.3 g, 58.4 mmol) and 7-azaindole (3.28 g, 27.8 mmol) were added and the mixture was heated at reflux for another 48 h, cooled, filtered, and concentrated. SGC (5% and 10% EtOAc-hexane) of the residue gave the title product as a colorless solid. Yield 2.8 g, 43%. 1H NMR (CDCI3) delta 8.37 (br, 1H), 7.96 (d, 1H, J = 7.5 Hz), 7.86 (s, 1H), 7.80 (d, 1H, J = 8.3 Hz), 7.71 (d, 1H, J = 8.3 Hz), 7.51 (d, 1H1 J = 3.7 Hz), 7.17 (br, 1H)1 6.67 (br, 1H), 2.62 (s, 3H). MS (AP+) m/e 234 (MH+).

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.

114897-91-5, name is 2-(4-Bromo-2-fluorophenyl)acetonitrile, 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. name: 2-(4-Bromo-2-fluorophenyl)acetonitrile

(4-Bromo-2-fluoro-phenyl)-acetonitrile (0.255 g, 1.19 mmol), PdCl2(dppf).CH2Cl2 (0.039 g, 0.048 mmol) and N-{2-hydroxy-2-[4(4,4,5,5-tetramethyl-[1,3,2]dioxaboralan-2-yl)phenyl]propyl}-2-propanesulfonamide (0.383 g, 1.0 mmol) are mixed together in dry DMF (30 mL) under N2 at ambient temperature. To this stirred mixture is added 2M Na2CO3 (1.25 mL, 2.5 mmol) and the resulting mixture is heated and stirred at 80 C. for 6 h. The mixture is cooled and poured into EtOAc. The EtOAc is extracted several times with H2O, washed with brine, dried (MgSO4), filtered, and the filtrate evaporated in vacuo. Chromatography on silica gel eluting with EtOAc/hexane gives the intermediate title compound.

The synthetic route of 114897-91-5 has been constantly updated, and we look forward to future research findings.

Related Products of 1187-42-4, 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. 1187-42-4 name is Diaminomaleonitrile, 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.

General procedure: AlCl3 (15 molpercent) was added to a solution of DAMN (1 mmol), ketone (1 mmol) and isocyanide (1 mmol), in 5 ml of CH3CN. The resulting mixture was stirred for an appropriate time at room temperature. After completion of the reaction, as indicated by thin-layer chromatography (TLC; ethyl acetate=n-hexane 3=1), the product was precipitated by addition of 10 ml of water. The precipitate was filtered off, washed with water, and then recrystallized from acetone. In the case of aromatic aldehyde, precipitate after filtration was loaded on column chromatography with 20percent ethyl acetate?hexane as an eluent system to furnish the product.

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

886498-08-4, name is 2-Fluoro-5-(trifluoromethoxy)benzonitrile, 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. Safety of 2-Fluoro-5-(trifluoromethoxy)benzonitrile

2-fluoro-5-(trifluoromethoxy)benzylamine-d2: To a mixture of2-fluoro-5-(trifluoromethoxy)benzonitrile (374 mg, 1.823 mmol) and sodium borodeuteride (176 mg, 4.19 mmol) in THF (10 mL) at 0 C was added over 45 mm, iodine (463 mg, 1.823 mmol) as a solution in 4 ml THF. The reaction mixture was heatedat reflux for 2 h. After cooling to 0 C, 6 N HC1 (2 ml) was carefully added. This mixture was heated at reflux for 30 mm. After cooling to rt, the mixture was partitioned between EtOAc (40 mL) and 1 N NaOH (40 mL). The organic layer was washed with water (20 mL) and brine (20 mL). After drying over anhydrous sodium sulfate, the organic layer was filtered and concentrated to afford2-fluoro-5-(trifluoromethoxy)benzylamine-d2 (385 mg, 1.823 mmol, 100 % yield)

The synthetic route of 886498-08-4 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. 78473-00-4, name is 4-Amino-3,5-dichlorobenzonitrile, This compound has unique chemical properties. The synthetic route is as follows., Recommanded Product: 4-Amino-3,5-dichlorobenzonitrile

To a solution of 4-amino-3,5-dichlorobenzonitrile (2.00 g, 10.63 mmol) in acetonitrile (12 ml) was added dropwise tetrafluoroboric acid (2.80 ml, 21.27 mmol). After stirring for 10 min, isoamyl nitrite (1.50 ml, 10.63 mmol) was added and the reaction mixture was cooled to 0 C. After a further 10 min, diethyl ether (50 ml) was added and the resulting precipitate was collected by filtration and dried to give the titled compound (1.9 g). 1H-NMR (D2O): 8.36-8.40 (2H)

According to the analysis of related databases, 78473-00-4, 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. 19924-43-7, name is 2-(3-Methoxyphenyl)acetonitrile, A new synthetic method of this compound is introduced below., Quality Control of 2-(3-Methoxyphenyl)acetonitrile

Step 1: 2-(3-Methoxyphenyl)-2-methylpropionitrile To a solution of (3-methoxyphenyl)-acetonitrile (8.0 g, 0.054 mol) in DMF (25 ml) cooled to 0 C., NaH (1.3 g, 0.054 mol) was added. The reaction was stirred for 30 min, and MeI (3.3 mL, 0.054 mol) was added. The reaction was stirred 1 h at room temperature. After this period, the reaction mixture was cooled again to 0 C., NaH (1.3 g, 0.054 mol) was added followed by MeI (3.3 ml, 0.054 mol) after 30 minutes. The reaction was stirred at room temperature overnight. DMF was evaporated and the crude diluted with brine and extracted with Et2O. The organic phase was washed with water, dried over Na2SO4, the solvent was evaporated under reduced pressure and the residue was purified by flash chromatography (petroleum ether:AcOEt 95:5) to give the title compound (4 g, 42% yield) as a colourless oil. ESI+MS: calcd for C11H13NO: 175.23; found: 176.1 (MH+).

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.