Month: May 2021

Synthetic Route of 149793-69-1,Some common heterocyclic compound, 149793-69-1, name is 3-Fluoro-5-(trifluoromethyl)benzonitrile, molecular formula is C8H3F4N, 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.

Step 1: 3-{[3-(Dimethylamino)propyl](methyl)amino}-5-(trifluoromethyl)benzonitrile 500 mg (2.64 mmol) of 3-fluoro-5-(trifluoromethyl)benzonitrile, 338 mg (2.91 mmol) of N,N,N’-trimethylpropane-1,3-diamine and 767 mg (5.52 mmol) of potassium carbonate in 5.0 ml of DMSO were stirred at 110 C. for 8 h. The reaction mixture was then separated directly into its components by preparative HPLC (Method 12). The product fractions were freed from the solvent, the residue was suspended in ethyl acetate and the suspension was washed successively with saturated aqueous potassium carbonate solution and saturated aqueous sodium chloride solution. The organic phase was dried over sodium sulphate and concentrated. This gave 290 mg (38% of theory) of the title compound. 1H NMR (400 MHz, DMSO-d6, delta/ppm): 7.38 (s, 1H), 7.31 (s, 1H), 7.21 (s, 1H), 3.44 (t, 2H), 2.97 (s, 3H), 2.18 (t, 3H), 2.12 (s, 6H), 1.62 (quint, 2H). LC/MS (Method 3, ESIpos): Rt=0.72 min, m/z=286 [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 3-Fluoro-5-(trifluoromethyl)benzonitrile, its application will become more common.

34667-88-4, name is 2-Fluoro-4-nitrobenzonitrile, 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 C7H3FN2O2

Reference Example 114 4-Amino-2-fluorobenzonitrile To a solution of 2-fluoro-4-nitrobenzonitrile (2.51 g) in methanol (125 mL) was added 10% palladium carbon (50% containing water, 237 mg), and the mixture was stirred under a hydrogen atmosphere for 3 hr. The reaction mixture was filtrated, and the filtrate was concentrated under reduced pressure. The residue was purified by basic silica gel column chromatography (eluent: hexane-ethyl acetate=1:1) to give the title compound as a pale-yellow solid (yield 1.43 g, 70%). 1H-NMR (CDCl3)delta: 4.31 (2H, brs), 6.37-6.45 (2H, m), 7.31-7.36 (1H, m).

The synthetic route of 34667-88-4 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. 868-54-2, name is 2-Aminoprop-1-ene-1,1,3-tricarbonitrile, A new synthetic method of this compound is introduced below., name: 2-Aminoprop-1-ene-1,1,3-tricarbonitrile

General procedure: Et3N (0.3 mmol) was added to a stirred solution of salicylaldehyde (3 mmol), 2-aminoprop-1-ene-1,1,3-tricarbonitrile (3 mmol) and 3-trifluoromethyl-2-pyrazolin-5-one in 5 ml of n-PrOH at ambient temperature. Then mixture was refluxed for 4 h. After the reaction was finished and cooled the solid was filtered and dried to isolate pure substituted 2,4-diamino-5-(5-hydroxy-3-(trifluoromethyl)-1H-pyrazol-4-yl)-5H-chromeno[2,3-b]pyridine-3-carbonitrile. In some cases cristallisation from EtOH-DMSO is needed.

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.

70591-86-5, name is 3-Bromobenzoylacetonitrile, 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 3-Bromobenzoylacetonitrile

Example IV-34 3-(3-bromophenyl)-5-isoxazolamine To a solution of 3-(3-bromophenyl)-3-oxopropanenitrile (1.12 g; 5.00 mmol; Note 1) in EtOH (20 mL) was added a solution of hydroxylamine hydrochloride (1.74 g; 25 mmol) and NaOAc (2.46 g; 30 mmol) in water (20 mL). The mixture was heated under reflux for 1 h, cooled and concentrated in vacuo. The residue was slurried in 1N NaOH and extracted with Et2O (*1). The organic layer was washed (water, brine), dried over Na2SO4 and concentrated in vacuo affording the title compound as a pale yellow solid which was used without further purification. LC/MS (method B) 2.21 min, m/z 239, 241 (Br isotopes).

The synthetic route of 70591-86-5 has been constantly updated, and we look forward to future research findings.

Related Products of 6629-04-5, The chemical industry reduces the impact on the environment during synthesis 6629-04-5, name is N-Cyanoacetylurethane, I believe this compound will play a more active role in future production and life.

To a stirred and cooled (5-10 C.) mixture of 5.6 parts of 4-amino-alpha-(4-chlorophenyl)-2-methoxybenzeneacetonitrile, 6.2 parts of concentrated hydrochloric acid and 50 parts of acetic acid is added dropwise, during a 15 minutes period, a solution of 1.25 parts of sodium nitrite in 10 parts of water at about 10 C. Upon completion, the whole is stirred for 60 minutes and then 3.6 parts of anhydrous sodium acetate and 2.8 parts of ethyl (2-cyanoacetyl)carbamate are added and stirring is continued for 2 hours at room temperature. The reaction mixture is poured into 250 parts of water. The product is filtered off, washed with water and dissolved in a mixture of trichloromethane and methanol (90:10 by volume). The organic layer is dried, filtered and evaporated. The residue is purified by column chromatography over silica gel using a mixture of trichloromethane and methanol (95:5 by volume) as eluent. The pure fractions are collected and the eluent is evaporated in vacuo, yielding ethyl [2-[[4-[(4-chlorophenyl)cyanomethyl]-3-methoxyphenyl]hydrazono]-2-cyanoacetyl]carbamate.

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, N-Cyanoacetylurethane, 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. 621-50-1, name is 2-(3-Nitrophenyl)acetonitrile, This compound has unique chemical properties. The synthetic route is as follows., Application In Synthesis of 2-(3-Nitrophenyl)acetonitrile

Example 5 Preparation of N-[3-(4,5-dihydro-1H-imidazol-2-ylmethyl)-phenyl]-methanesulfonamide hydrochloride STR112 1-Chloromethyl-3-nitro-benzene (5 g) and 4.28 g of sodium cyanide were dissolved in a mixture of 15 ml of water and 50 ml of dioxane and the two phase mixture was heated to 100 C. for 12 hr. The dioxane was removed by evaporation and the aqueous solution was extracted with dichloromethane. The organic extract was washed with brine, dried, and evaporated. The residue was purified by flash column chromatography eluding with EtOAc:hexane (1:4) to afford 2.86 g of a tan solid, mp 51.7-52.7 C., of (3-nitro-phenyl)-acetonitrile. STR113 (3-Nitro-phenyl)-acetonitrile (2.79 g) was dissolved in 50 ml of ethyl acetate and the mixture was treated with 19.5 g of tin (II) chloride dihydrate and stirred at room temperature for 72 hr. The mixture was diluted with ethyl acetate and treated with saturated sodium bicarbonate solution, separated, and extracted with ethyl acetate. The extracts were combined, dried, and evaporated, leaving 2.1 g of tan oil of (3-amino-phenyl)-acetonitrile. STR114

According to the analysis of related databases, 621-50-1, the application of this compound in the production field has become more and more popular.

Related Products of 77326-36-4, 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. 77326-36-4, name is 2-Amino-6-fluorobenzonitrile, This compound has unique chemical properties. The synthetic route is as follows.

To a solution of 2-ethylbutan-l-ol (1.02 g, 10.0 mmol) in dry THF (60 mL) was carefully added NaH (60% in mineral oil, 480 mg, 12.0 mmol) in small portions at 0 C under nitrogen. The reaction mixture was stirred at 0 C under nitrogen for 2 hrs. To this solution was added 2- amino-6-fluorobenzonitrile (1.36 g, 10.0 mmol), and the reaction solution was stirred at 0 C – RT for 2 hrs, and then at 65 C overnight under nitrogen. The reaction was cooled down to room temperature then quenched with brine, and extracted with EtOAc (3X). The combined organic layers were washed with brine, dried over Na2S04. Filtered and evaporated under reduced pressure. The residue was purified by chromatography on silica gel (eluent: 20% EtOAc in hexanes) to give the title compound as colorless oil (1.29 g, 59%). 1H NMR (400 MHz, CDC13) delta 0.93 (t, J= 8 Hz, 6H), 1.55-1.43 (m, 4H), 1.73- 1.65 (m, 1H), 3.90 (d, J= 4 Hz, 2H), 4.10 (brs, 2H), 6.25 (d, J = 8 Hz, 1H), 6.34 (d, J = 8 Hz, 1H), 7.20 (t, J = 8 Hz, 1H).

The chemical industry reduces the impact on the environment during synthesis 2-Amino-6-fluorobenzonitrile. I believe this compound will play a more active role in future production and life.

151-18-8, name is 3-Aminopropanenitrile, 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: 3-Aminopropanenitrile

To a suspension of (S)-3-((tert-butoxycarbonyl)amino)-5-methyl-4-oxo-2,3,4,5- tetra-hydrobenzo[b][l,4]oxazepine-7-carboxylic acid (185.0 mg, 0.550 mmol) in DCM (5.0 mL) was added l-chloro-N,N,2-trimethylprop-l -en- 1 -amine (88 mg, 0.660 mmol) as a solution in DCM (0.10 ml) dropwise over 1 min. The reaction mixture was stirred at rt for lh and became a homogeneous solution. The reaction mixture was cooled in an ice-bath then 3-aminopropanenitrile (154 mg, 2.200 mmol) was added dropwise as a solution in DCM (0.25 mL). After 10 min, the ice-bath was removed then 10 % aq citric acid solution was added and the mixture was stirred vigorously for 15 min . The organic phase was separated, washed with sat. aq sodium bicarbonate, brine then dried over Na2S04and concentrated in vacuo. The residue was purified by FCC [EtO Ac-Hex: 45-80%] to yield the desired product (190.0 mg, 89%).MS (m/z) 389.3 (M+H+).

The synthetic route of 151-18-8 has been constantly updated, and we look forward to future research findings.

Application of 50846-36-1, 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. 50846-36-1, name is 2-Amino-2-methylpropanenitrile hydrochloride, This compound has unique chemical properties. The synthetic route is as follows.

To a stirred mixture of 3-(2-(4-fluorophenyl)-3-(methylcarbamoyl)-6-(2,2,2- trifluoroethoxy) benzofuran-5-yl)benzoic acid (40 mg, 0.082 mmol) and 2-amino-2- methylpropanenitrile hydrochloride (9.90 mg, 0.082 mmol) in DMF (2.5 mL) at room temperature under a N2 atmosphere was added DIPEA (0.072 mL, 0.410 mmol). The mixture was cooled to 0C, and HATU (46.8 mg, 0.123 mmol) was added to the mixture, and then stirring was continued at r.t for 16 hr. After completion of the reaction, the mixture was diluted with water and the product extracted with EtOAc (25 ml x 3). The combined organic layers were washed with saturated brine solution, dried over Na2S04, filtered and concentrated under reduced pressure. The crude solid product was purified by Prep HPLC to obtained 5-(3-((2-cyanopropan-2- yl)carbamoyl)phenyl)-2-(4-fluorophenyl)-N-methyl-6-(2,2,2- trifluoroethoxy )benzofuran-3-carboxamide as a white solid. Yield: 12.00 mg, (26.40 %). PREPARATIVE HPLC: Column: X-BRIDGE C-18(19* 150)mm*5u, Mobile Phase: lOmM Ammonium acetate (A): MeCN (B), Flow: 15 ml/min, Rt: 10.38 min. 1H NMR (400 MHz, CHLOROFORM-d) delta ppm = 7.93 – 7.84 (m, 4 H), 7.82 (s, 1 H), 7.72 – 7.69 (m, 1 H), 7.56 – 7.51 (m, 1 H), 7.20 (t, J= 8.7 Hz, 2 H), 7.14 (s, 1 H), 6.22 (s, 1 H), 5.84 (bs, 1H), 4.36 (q, J= 8.1 Hz, 2 H), 3.01 (d, J= 4.9 Hz, 3 H), 1.84 (s, 6 H). 19F NMR (376.6 MHz, CHLOROFORM-d) delta: -73.38, -109.44. LCMS: (ES+) m/z = 554.2 (M+H)+, Column-Acentis Express C18 (50 x 2.1 mm; 2.7 urn), Buffer : lOmM Ammonium Formate in Water pH 4.5, Mobile phase A: Buffer : MeCN (98 : 2), Mobile phase B: Buffer : MeCN (2 : 98), Flow: l .Oml/min. Rt: 2.18 min, wavelength: 220nm. HPLC Method: SUNFIRE (150 X 4.6mm) 3.5micron, Buffer: 0.05% TFA in water, Mobile Phase A: Buffer: MeCN (95:5), Mobile Phase B: MeCN: Buffer (95:5), Flow: 1.0 ml/min, Wavelength: 254 nm, Rt: 19.37 min, Wavelength: 220 nm, Rt: 19.37 min. HPLC Method: XBridge Phenyl (150 X 4.6mm) 3.5micron SC/749, Buffer: 0.05% TFA in water, Mobile Phase A: Buffer: MeCN (95:5), Mobile Phase B: Buffer: MeCN (5:95), Flow: 1.0 ml/min, Wavelength: 254 nm, Rt: 17.00 min, Wavelength: 220 nm, Rt: 17.00 min.

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

Related Products of 127946-77-4, The chemical industry reduces the impact on the environment during synthesis 127946-77-4, name is 1-Amino-1-cyclopropanecarbonitrile hydrochloride, I believe this compound will play a more active role in future production and life.

E. Synthesis of the Intermediate Amide 6H The carboxylic acid 5A (195 mg, 0.5 mmol), 1-aminocyclopropanecarbonitrile hydrochloride (65.2 mg, 550 mumol), HATU (380 mg, 1.00 mmol) and ethyldiisopropyl amine (262 muL, 1.5 mmol) were dissolved in acetonitrile (10 mL) and stirred at room temperature over night. The reaction was concentrated under reduced pressure. The residue was diluted with 5% aqueous sodium carbonate solution and extracted twice with ethyl acetate. The combined organic layers were washed with 1M aqueous hydrogen chloride solution and with saturated aqueous sodium chloride solution, dried over Na2SO4, filtered and concentrated under reduced pressure to yield (2S,4R)-tert-butyl 4-(2-chlorophenylsulfonyl)-2-(1-cyanocyclopropylcarbamoyl)-pyrrolidine-1-carboxylate 6H as a yellow oil (66%). MS ISP (m/e): 354.2 (100) [(M-BOC+H)]+, 398.1 (25) [(M-Isobutylene+H)]+, 454.1 (12) [(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, 1-Amino-1-cyclopropanecarbonitrile hydrochloride, other downstream synthetic routes, hurry up and to see.