Tag: M.W=100-200

127946-77-4, name is 1-Amino-1-cyclopropanecarbonitrile hydrochloride, 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. Computed Properties of C4H7ClN2

To a vial containing (lR,2R,5S)-2-(2-(ieri-butyl)-5-(4-(l-imino-l- oxidothiomorpholino)phenyl)oxazol-4-yl)-5-fluorocyclohexanecarboxylic acid (12 mg, 0.025 mmol) was added 1-aminocyclopropanecarbonitrile hydrochloride (72.5 mg, 0.61 1 mmol), DIPEA (1 15 uL, 0.696 mmol), and HATU (13.4 mg, 0.035 mmol). The resulting mixture was heated at 65 C for 4.5 hours. The reaction mixture was cooled to RT. The crude mixture was purified directly via reverse phase preparative HPLC (water/10 to 75% MeCN, 0.1 % TFA, 15 min). Fractions with the desired product after HPLC were treated with saturated NaHCC>3 and extracted with CH2CI2 (3 x 10 mL), then EtOAc, washed with brine (30 mL), dried (MgS04), and evaparated under reduced pressure giving 8.2 mg (60%) of (2R,5S)-2-(2-(/er/-butyl)-5-(4-(l-imino-l – oxidothiomorpholino)phenyl)oxazol-4-yl)-N-(l -cyanocyclopropyl)-5- fiuorocyclohexanecarboxamide (Compound 13).1H NMR (500 MHz, CDCl3): delta 0.89-0.84 (m; 2 H); 0.98-0.93 (m; 1 H); 1.33-1.28 (m; 1 H); 1.41-1.39 (m; 1 H); 1.43 (s; 9 H); 2.07-1.92 (m; 3 H); 2.15 (br t; J = 16.14 Hz; 2 H); 2.99 (t; J = 1 1.59 Hz; 1 H); 3.17-3.13 (m; 5 H); 3.94-3.86 (m; 4 H); 5.00 (d; J = 47.85 Hz; 1 H); 6.35 (s; 1 H); 6.95 (d; J = 8.51 Hz; 2 H); 7.46 (d; J = 8.47 Hz; 2 H); MS (ES, m/z): 542.2 (M + 1)

The synthetic route of 127946-77-4 has been constantly updated, and we look forward to future research findings.

Some common heterocyclic compound, 4210-32-6, name is 4-(tert-Butyl)benzonitrile, molecular formula is C11H13N, 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-(tert-Butyl)benzonitrile

General procedure: To a solution of adiponitrile (219 muL, 1.95 mmol) and the appropriate mononitrile (1.30 mmol) in p-xylene (1 mL) in a carousel tube was added t-BuOK (29.2 mg, 0.26 mmol) in one portion. The reaction vessel was heated in a carousel to 120 °C for 4 h. After cooling to room temperature, CH2Cl2 (ca. 30 mL) was used to transfer the mixture onto a silica cartridge for purification.

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 4210-32-6, its application will become more common.

Reference 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.

A 2 L, three-neck, round-bottom flask equipped with overhead stirring, a thermocouple, N2 inlet/outlet was charged with Int. 7 (75.0 g, 0.239 mol, 1 wt), acetic acid (600 mL, 8 vol), water (150 mL, 2 vol), and concentrated HC1 (71.3 mL, 0.95 vol). The resulting thin slurry was cooled to 6 C and a solution of NaN02 (16.8 g, 0.243 mol, 1.02 equiv) in water (37.5 mL, 0.5 vol) was added over a period of 10 min while maintaining a batch temperature below 10 C. After an additional 10 min of agitation between 5-10 C,HPLC analysis showed complete conversion of Int. 7 to the diazonium intermediate. A solution of NaOAc (54.5 g, 0.664 mol, 2.78 equiv) in water (225 mL, 3 vol) was added over a period of 6 min while maintaining a batch temperature below 10 C. N-cyanoacetylurethane (37.9 g, 0.243 mol, 1.02 equiv) was immediately added, the cooling was removed, and the batch naturally warmed to 8 C over 35 min. HPLC analysis showed complete consumption of the diazonium intermediate and the reaction was deemed complete. The batch warmed naturally to 21 C and was filtered through Sharkskin filter paper. The reactor and cake were washed sequentially with water (375 mL, 5 vol) twice. The collected orange solid was dried in a 35 C vacuum oven for 64 h to provide crude Int. 8 (104.8 g, 91%). A I L, three-neck, round-bottom flask equipped with overhead stirring, a thermocouple, and N2 inlet/outlet was charged with crude Int. 8 (104.4 g, 1 wt) and acetic acid (522 mL, 5 vol). The resulting slurry was heated to 50 C and held at that temperature for 1.5 h. The batch cooled naturally to 25 C over 2 h and was filtered through Sharkskin filter paper. The reactor and cake were washed sequentially with water (522 mL, 5 vol) and the cake conditioned under vacuum for 1.75 h. The light orange solid was dried to constant weight in a 40 C vacuum oven to provide 89.9 g (78% from Int. 7) of the desired product. 1H NMR (DMSO) was consistent with the assigned structure.

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.

Application of 23842-82-2, 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 23842-82-2 as follows.

General procedure: Matrine 1 (1.24 g, 5 mmol) dissolved in DCM (30 mL) was treatedwith POCl3 (2 eq., 10 mmol) at room temperature. When color of thereaction mixture turned yellow, it was then stirred at 60 C for 2-3 h.The solution was then cooled to room temperature and the correspondinganiline bearing cyan derivatives 18a-h (1-1.5 eq.) dissolvedin DCM were added dropwise, followed by reflux for 12 h at 60C. Afterreaction completion, NaOH aqueous was added to adjust the pH to 8-9.The mixture was then extracted with DCM (3 × 20 mL). The organiclayers were collected, dried over MgSO4, and concentrated. The residuewas purified by column chromatography to obtain product 20a-h.

According to the analysis of related databases, 23842-82-2, the application of this compound in the production field has become more and more popular.

Electric Literature of 2698-41-1, 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. 2698-41-1, name is 2-(2-Chlorobenzylidene)malononitrile, This compound has unique chemical properties. The synthetic route is as follows.

General procedure: A mixture of hydrazine hydrate (1.5 mmol, 80%),ethyl acetoacetate (1 mmol), aromatic aldehydes (1mmol), malononitrile (1 mmol) and starch solution(4 mL), was stirred at desired temperature for 60-90 min. Progress of the reaction was monitored by TLC. After completion of the reaction, the reaction mixture was cooled to RT and diluted with water. The reaction mixture was filtered for the separation of product. The crude product was purified by recrystallization from ethanol to afford pure products in excellent yield.After removal of the extra added (for work-upprocess) water from the filtered solution, the starchsolution (4 mL) is recovered and reused for thesubsequent reaction.

The chemical industry reduces the impact on the environment during synthesis 2-(2-Chlorobenzylidene)malononitrile. I believe this compound will play a more active role in future production and life.

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. 42872-74-2, name is 3-Bromo-4-methylbenzonitrile belongs to nitriles-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below. Application In Synthesis of 3-Bromo-4-methylbenzonitrile

A solution of 3-bromo-4-methylbenzonitrile (1 g), acetamidine hydrochloride (714 mg), cesium carbonate (5 g) and copper (I) bromide (36 mg) in dry dimethyl sulfoxide (25 mL) was stirred at 120 C. for 3 h. The mixture was chilled, diluted with EtOAc (200 mL) and washed with water. The organic layer was dried and the volatiles were removed under reduced pressure. The residue was purified by chromatography (SiO2, 150 g, DCM/MeOH) to yield the desired product (36% yield). LC-MS (Method 1): m/z [M+H]+=252.1 (MW calc.=252.11); Rt=3.5 min.

The synthetic route of 42872-74-2 has been constantly updated, and we look forward to future research findings.

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. 67515-59-7, name is 4-Fluoro-3-(trifluoromethyl)benzonitrile belongs to nitriles-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below. SDS of cas: 67515-59-7

A mixture of 4-fluro 3-trifluro-methylbenzonitrile (5 g, 26.4 mmol) and 2-methylpiperidine (6.25 ml_, 52.9 mmol) was heated at 10O C under N2 for 12h.The reaction mixture was diluted with water (100 ml_) and was extracted with EtOAc (2chi100ml_). The organic layer was washed with water (2chi100mL) and brine solution (10OmL). The solvent was dried over sodium sulphate and concentrated. The residue was purified by flash chromatography using silica-gel (60-120 mesh) and pet-ether /EtOAc as eluent to afford the title compound as an off-white solid. 1H NMR (CDCI3, 400 MHz) delta 7.87 (s, 1 H), 7.71 -7.74 (d, 1 H), 7.50 (bs, 1 H), 2.95-3.03 (m, 2H), 2.49-2.54 (m, 1 H), 1.71 -1 .77 (m, 3H), 1 .58-1.59 (m, 1 H), 1.36-1.39 (m, 2H), 0.75-0.77 (d, 3H). HPLC (Method C) Rt 5.09 min (Purity: 98.8%).

The synthetic route of 67515-59-7 has been constantly updated, and we look forward to future research findings.

Adding a certain compound to certain chemical reactions, such as: 268734-34-5, name is Methyl 4-cyano-3-fluorobenzoate, 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 268734-34-5, COA of Formula: C9H6FNO2

EXAMPLE 52B 2-fluoro-4-(hydroxymethyl)benzonitrile A solution of Example 52A (1.0 g, 5.58 mmol) in THF (20 mL) at room temperature was treated with a solution of CaCl2 (1.24 g, 11.16 mmol) in ethanol (20 mL). The resulting solution was treated with NaBH4 (845 mg, 22.33 mmol) over 20 minutes, stirred for 1.25 hours, then slowly quenched with saturated ammonium chloride (100 mL), and concentrated. The remaining aqueous portion was extracted with ethyl acetate (3*100 mL) and the combined extracts were dried (MgSO4), filtered, and concentrated to provide the desired product. MS (APCI) m/z 169 (M+NH4)+; 1H NMR (300 MHz, CDCl3) delta7.60 (t, 1H), 7.29-7.23 (m, 2H), 4.80 (s, 2H).

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, Methyl 4-cyano-3-fluorobenzoate, other downstream synthetic routes, hurry up and to see.

Adding a certain compound to certain chemical reactions, such as: 35202-54-1, name is 4,5-Dimethoxy-1-cyanobenzocyclobutane, 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 35202-54-1, name: 4,5-Dimethoxy-1-cyanobenzocyclobutane

EXAMPLE 4 (R,S)-3,4-Dimethoxy-bicyclo[4.2.0]octa-4,3,5-triene-7-carbaldehyde 10 g (52.8 mmol) of 3,4-dimethoxy-bicyclo[4.2.0]octa-1,3,5-triene-7-carbonitrile are dissolved in 100 ml of anhydrous toluene. The solution is cooled to -78° C. and then 55 ml of diisobutylaluminum hydride solution (1.2M in toluene) are added dropwise while maintaining the temperature below -65° C. (addition time=45 minutes). Stirring is carried out for 1 hour at -78° C. once the addition is complete. Hydrolysis is carried out by adding dropwise 20 ml of methanol. The temperature is allowed to return to -30° C. and then the reaction mixture is added to 200 ml of HCl (0.1N) and extraction with ether is carried out twice. The organic phase is washed in succession with water and saturated aqueous NaCl solution and then dried over MgSO4, filtered and evaporated to dryness to obtain 8 g of title product in the form of pale yellow oil. Yield=79percent IR (pure): nu=2714, 2630, 1712 cm-1.

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, 4,5-Dimethoxy-1-cyanobenzocyclobutane, other downstream synthetic routes, hurry up and to see.

These common heterocyclic compound, 1080-74-6, name is 2-(3-Oxo-2,3-dihydro-1H-inden-1-ylidene)malononitrile, 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-(3-Oxo-2,3-dihydro-1H-inden-1-ylidene)malononitrile

Then F (1.07 g, 1.5 mmol) was dissolved in chloroform.G (1.16g 6mmol) was added and 1mL of pyridine was added as a catalyst. The reaction was carried out at reflux temperature of chloroform for 12 hours. After the reaction was completed, water was added three times with dichloromethane, and the solvent such as dichloromethane was removed by rotary evaporation.The crude product was obtained and purified further by silica gel column chromatography.Using petroleum ether/dichloromethane 1:1 (v/v) as an eluent, a blue-black solid (1.41 g, yield 88%) was obtained as the object compound M2.

The synthetic route of 2-(3-Oxo-2,3-dihydro-1H-inden-1-ylidene)malononitrile has been constantly updated, and we look forward to future research findings.