Tag: M.W=100-200

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 64248-64-2 as follows. Product Details of 64248-64-2

EXAMPLE 37 N-(2-Cyano-4-fluorophenyl)-4-piperidone propylene ketal (39) A mixture of 2,5-difluorobenzonitrile (2.272 g, 16.33 mmol) and 4-piperidone propylene ketal (2.570 g, 16.34 mmol) was stirred at room temperature (11 d). The resulting mixture was diluted with dichloromethane and sodium carbonate solution and the aqueous layer was extracted with two additional portions of dichloromethane. The combined organic extracts were washed with brine and dried over Na2SO4. The solvent was removed in vacuo. PCTLC (SiO2, 6 mm, 20% EtOAc-80% hexane) afforded the title compound (39). 1H NMR (CDCl3, 400 MHz) consistent with assigned structure. FABLRMS m/e 277 g/mole (M++H, C15H17FN2O2=277 g/mole.) HPLC (Vydac; C18; diameter=4.6 mm; length=150 mm; gradient=H2O [0.1% H3PO4]-CH3CN, 95%-5%, 5%-95%, over 16 minutes, 2 ml/min flow rate) RT=7.31 min; focus=215 nm; 99.3% pure.

According to the analysis of related databases, 64248-64-2, the application of this compound in the production field has become more and more popular.

Reference:
Patent; Merck & Co., Inc; Synaptic Pharmaceutical Corporation; US6376503; (2002); B1;,
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Adding a certain compound to certain chemical reactions, such as: 4640-67-9, name is 3-(4-Fluorophenyl)-3-oxopropanenitrile, 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 4640-67-9, Computed Properties of C9H6FNO

To a solution of 3-(4-fluorophenyl)-3-oxopropanenitrile (1 g, 6.13 mmol) in ethanol (11 mL) was added hydrazine hydrate (1.82 mL, 36.8 mmol). The reaction mixture was stirred at 100C in a sealed vessel for 6 h. The solvents were evaporated in vacuo and the residue was extracted with EtOAc and brine. The organic solvents were dried over magnesium sulphate and evaporated in vacuo. The residue (1.18 g) was dissolved in EtOAc (anhydrous), then the procedure for Intermediate 1 was applied. The title compound (914 mg, 57%) was isolated as a white powder. C NMR delta (DMSO-d6, 75 MHz) 173.19, 163.01 (d, JCF 245.0 Hz), 154.61, 141.81, 141.59, 128.63 (2C, d, JCF 8.4 Hz), 127.97, 115.94 (2C, d, JCF 21.6 Hz), 86.88. MS (m/z) 263 [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, 3-(4-Fluorophenyl)-3-oxopropanenitrile, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; HORSLEY Helen Tracey; HUANG Qiuya; NEUSS Judi Charlotte; REUBERSON James Thomas; VANDERHOYDONCK Bart; WO2015/193169; A1; (2015);,
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Related Products of 67832-11-5, 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. 67832-11-5 name is 4-Bromo-2-methylbenzonitrile, 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 4-bromo-2-methylbenzonitrile (3 g, 15 mmol) in THF (20 mL) was added BH3¡¤THF (45 mL, 45 mmol) at 0 C. The solution was stirred for 1 h and heated to 80 C for 2 h. The mixture was quenched with H2O and extracted with EtOAc (50 mL x 3). The organic layer was concentrated in vacuo to afford a residue which was suspended in saturated HCl/EtOAc and filtered. The filter cake was washed with diethyl ether (20 mL x 3) and dried under vacuum to afford the desired product (2.1 g, yield 69%) as white solid. ESI-MS (M+H)+: 200.1.

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

Reference:
Patent; BIOGEN IDEC MA INC.; SUNESIS PHARMACEUTICALS, INC.; HOPKINS, Brian T.; MA, Bin; CHAN, Timothy Raymond; KUMARAVEL, Gnanasambandam; MIAO, Hua; BERTOLOTTI-CIARLET, Andrea; OTIPOBY, Kevin; WO2015/89327; (2015); A1;,
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Adding a certain compound to certain chemical reactions, such as: 654-70-6, name is 4-Cyano-3-trifluoromethylaniline, 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 654-70-6, name: 4-Cyano-3-trifluoromethylaniline

At room temperature, 1 ml of thiophosgene is added to 22 ml of water to form a suspension.Then 2.23 g of 4-amino-2-trifluoromethylbenzonitrile was added dropwise to the above solution.The dropwise addition time was 20 minutes, and after completion of the dropwise addition, stirring was continued for 1 hour at room temperature. After completion of the reaction, the reaction solution was extracted with 2 x 20 ml of methylene chloride. The organic phases were combined, dried over anhydrous sodium sulfate, filtered, and concentrated under reduced pressure (about 0.4 mmHg) to give 2.72 g of the title compound,Brown oil.

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

Reference:
Patent; Beijing Haimeiyuan Pharmaceutical Technology Co., Ltd.; Wang Yingzhao; Di Wei; Liu Yanling; (34 pag.)CN104341351; (2018); B;,
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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. 6609-57-0, name is 2-Ethoxybenzonitrile, A new synthetic method of this compound is introduced below., Computed Properties of C9H9NO

2-ethoxy benzonitrile (25g, 170 mmol) was added to an ice cold solution of chloro sulfonic acid (183.7g, 1.57mol) over a period of one hour. The temperature of the reaction mixture was maintained at about 5C to 7C. The reaction mixture was stirred at about 5C to 7C overnight. The reaction mass was added into ice water (500 mL) slowly at 100C to 15C. The suspension was stirred for about 1 hour, filtered under nitrogen atmosphere to obtain 5-chlorosulfonyl-2-ethoxy benzonitrile as yellow solid which was used directly in next step.

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:
Patent; RANBAXY LABORATORIES LIMITED; MITTAL, Anu; KHANNA, Mahavir, Singh; THAPER, Rajesh, Kumar; PRASAD, Mohan; WO2011/16016; (2011); A1;,
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Synthetic Route of 63069-50-1, The chemical industry reduces the impact on the environment during synthesis 63069-50-1, name is 4-Amino-3-fluorobenzonitrile, I believe this compound will play a more active role in future production and life.

EXAMPLES 11-28Synthesis of Examples 11-28 were prepared following General Procedures l-lll. General Procedure I. Preparation of Dimethylamino Compounds 2a-iTo mixture of 1a-i (1 mmol) and NaH (2.6 mmol) in anhydrous THF (4 ml.) was added CH3I (2.6 mmol). The reaction mixture was stirred at room temperature for 3-12 hours, monitoring by TLC. The reaction was quenched by adding small amount of CH3OH, then H2O, the mixture was then concentrated and extracted three times with EtOAc. The combined extracts were washed with H2O, then dried over Na2SO4. Separation and purification (hexane/EtOAc = 10:1 or 10:2) gave the following compounds. 4-Dimethylamino-3-fluoro-benzonitrile, MS: m/z 165 (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, 4-Amino-3-fluorobenzonitrile, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; WYETH; WO2009/120826; (2009); A1;,
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A common compound: 4110-35-4, name is 3,5-Dinitrobenzonitrile, belongs to nitriles-buliding-blocks compound, it can change the direction of chemical reaction, and react with certain compounds to generate new functional products. A new synthetic method of this compound is introduced below. 4110-35-4

Example 137Alternative Preparation of 3-(4,5-dihydro-4-methyl-5-oxotetrazol-1-yl)-5-nitrobenzonitrileA mixture of 3,5-dinitrobenzonitrile (386 mg, 2.0 mmol), 1-methyl-1H-tetrazol-5(4H)-one (400 mg, 4.0 mmol) and K2CO3 (552 mg, 4.0 mmol) in NMP (6 mL) was heated to 110 C. and stirred overnight. After allowing to cool, the mixture was poured in to H2O (75 mL) and EtOAc (40 mL). The aqueous and organic layers were partitioned and the aqueous layer was extracted with EtOAc (2¡Á30 mL). The combined organic extracts were washed with brine (1¡Á20 mL), dried (Na2SO4), filtered and the solvent removed under vacuum to leave a crude residue. The residue was purified by column chromatography on silica gel using EtOAc/hexane (3:7 to 4:6) as eluent to give the product (182 mg, 37%) as a solid.Data identical to previously synthesized material. (Example 136)Note: 1-methyl-1H-tetrazol-5(4H)-one was prepared according to procedure detailed in EP643049 (1995); Preparation of 1-substituted-5(4H)-tetrazolinones by desulfurization of tetrazolinethiones, which is hereby incorporated by reference.

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, 4110-35-4, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; Singh, Rajinder; Tso, Kin; Zhang, Jing; Duncton, Matthew; Alvarez, Salvador; Kolluri, Rao; Ramphal, John; Holland, Sacha; US2011/130415; (2011); A1;,
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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. 127946-77-4 name is 1-Amino-1-cyclopropanecarbonitrile hydrochloride, 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. 127946-77-4

(3R,4R)-N-( 1 -Cyanocyclopropyl)-4-(5 -(4-( 1,1 -dioxidothiomorpholino)phenyl)-2-(5 – fluoropyridin-3 -yl)thiazol-4-yl)bicyclo [4.1 . 0]heptane-3 -carboxamide was synthesized following the same procedure as in Step H of Example 1 using (3R,4R)-4-(5-(4-(1,1- dioxidothiomorpholino)phenyl)-2-(5 -fluoropyridin-3 -yl)thiazol-4-yl)bicyclo [4.1 . 0]heptane-3 -carboxylic acid (0.180 g, 0.340 mmol, 1.00 equiv), DMF (5 mL), 1- aminocyclopropanecarbonitrile hydrochloride (0.202 g, 1.70 mmol, 5.00 equiv), HATU (0.324 g, 0.850 mmol, 2.50 equiv) and DIPEA (0.330 g, 2.55 mmol, 7.48 equiv). This resulted in 0.135 g (67%) of (3R,4R)-N-( 1 -Cyanocyclopropyl)-4-(5 -(4-( 1,1 -dioxidothiomorpholino)phenyl)-2-(5 – fluoropyridin-3-yl)thiazol-4-yl)bicyclo[4. 1 .0]heptane-3-carboxamide as a yellow solid: MS (ES,m/z): 592.1 (M + 1).

At the same time, in my other blogs, there are other synthetic methods of this type of compound, 1-Amino-1-cyclopropanecarbonitrile hydrochloride, and friends who are interested can also refer to it.

Reference:
Patent; MERCK SHARP & DOHME CORP.; STACHEL, Shawn; PAONE, Daniel, V.; LI, Jing; GINNETTI, Anthony; LIM, John; FU, Jianmin; XU, Shimin; WO2015/54038; (2015); A1;,
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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. 60899-34-5, name is 1-Oxo-2,3-dihydro-1H-indene-4-carbonitrile belongs to nitriles-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below. 60899-34-5

PREPARATION 10 1-hydroxy-4-indanecarbonitrile (racemic) 1.46 g of 4-cyano-1-indanone in 131 ml of tetrahydrofuran is cooled to +5 C., 1 g of potassium borohydride is added in small fractions, with agitation for one hour 15 minutes, followed by pouring over 200 ml of water containing sodium chloride, and extraction with isopropyl ether. The organic phase is dried, brought to dryness under reduced pressure and the residue is chromatographed on silica in a hexane-ethyl acetate mixture (6-4). 1.40 g of expected product is obtained, M.p.=98 C.

The synthetic route of 60899-34-5 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Roussel Uclaf; US5180741; (1993); A;,
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These common heterocyclic compound, 612-24-8, name is 2-Nitrobenzonitrile, 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. 612-24-8

General procedure: A round bottom flask equipped with a magnetic stirrer bar was charged with the 2-nitroacylbenzene (1.00 mmol) in EtOAc-MeOH (1:1; 5 mL). SnCl2.H2O (3.00 mmol) was added and the reaction stirred at room temperature overnight. The reaction was partitioned between DCM (30 mL) and NaHCO3 (20 mL). The aqueous phase was extracted with DCM (3 ¡Á 10 mL) and the organic portions combined, washed with H2O (10 mL), saturated aqueous NaCl (10 mL), dried over MgSO4, filtered and reduced in vacuo. The residue was purified by column chromatography (SiO2, hexane/EtOAc) to provide the title compound. General procedure gave the title compound as an orange solid (116 mg, 87 %).

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 612-24-8.

Reference:
Article; Chauhan, Jay; Fletcher, Steven; Tetrahedron Letters; vol. 53; 37; (2012); p. 4951 – 4954;,
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