Tag: M.W=200-300

Related Products of 213598-11-9, 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. 213598-11-9, name is Methyl 3-cyano-4-isopropoxybenzoate belongs to nitriles-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

General procedure: 3-cyano-4-(propan-2-yloxy) benzoic acid: To a solution of methyl 3-cyano-4- (propan-2-yloxy)benzoate (5 g, 22.81 mmol, 1.00 equiv) in methanol/ water ( 30: 10 mL) was added sodium hydroxide (1.77 g, 2.30 equiv). The resulting solution was stirred for 2 h at 25 C. The pH value of the solution was adjusted to 3 with hydrogen chloride (1 Mol/L). The resulting solution was extracted with ethyl acetate (3 x 20 mL), and the organic layers were combined, dried over anhydrous sodium sulfate, concentrated under vacuum to afford 4.4 g of 3-cyano-4-(propan-2-yloxy) benzoic acid as a white solid.

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

Reference:
Patent; AUSPEX PHARMACEUTICALS, INC.; ZHANG, Chengzhi; CHAKMA, Justin; (91 pag.)WO2016/164180; (2016); 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. 1835-65-0, name is 3,4,5,6-Tetrafluorophthalonitrile belongs to nitriles-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below. SDS of cas: 1835-65-0

Referential Example 1 Synthesis of 4,5-bis(2,5-dichlorophenoxy)-3,6-difluorophthalonitrile Into a separable flask of glass provided with a stirrer, a thermometer, a water separation tube, and a cooling tube and having an inner volume of 300 ml, 242.5 gr of acetone and 19.1 gr (0.0955 mol) of tetrafluorophthalonitrile were placed, to dissolve tetrafluorophthalonitrile in acetone homogeneously. Next, the resultant solution and 134 gr (0.2306 mol) of potassium fluoride were added together and the resultant reaction slurry was retained at -5° C. To this reaction slurry, 34.1 gr (0.2092 mol) of 2,5-dichlorophenol dissolved uniformly in 30.5 gr of acetone was added dropwise over a period of one hour. The reaction proceeding during the dropwise addition was continued with the reaction product cooled from the exterior so as to keep the interior temperature thereof in the range of -5° C. to 0° C. After the dropwise addition was completed, the reaction mixture was retained for additional two hours. After the reaction was completed, the contents of the flask were cooled to 20° C. and filtered to separate the solid component. The solid component was washed with 10 gr of acetone and the washed solid component and the filtrate were mixed together. The resultant filtrate was evaporated under a reduced pressure to expel acetone by distillation. The weight of the produced dry component was 45.8 gr (crude yield: 98.7 mol). This dry component was found to contain 42.9 gr of the target product, 4,5-bis(2,5-dichlorophenoxy)-3,6-difluorophthalonitrile (yield: 92.4 mol percent).

The synthetic route of 1835-65-0 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Hirota, Kouichi; Hashimoto, Yukihide; Masuda, Kiyoshi; Kitao, Masunori; US2005/203293; (2005); A1;,
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Synthetic Route of 330792-69-3, 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. 330792-69-3, name is 2-(Methoxy(4-phenoxyphenyl)methylene)malononitrile, This compound has unique chemical properties. The synthetic route is as follows.

80% Hydrazine hydrate (32.5 ml) was added to a mixture of 2-(methoxy(4- phenoxyphenyl)methylene)malononitrile (48 gms) and methanol (192 ml) at 25-30C and stirred for 2 brs at the same temperature. Water was added to the reaction mixture at 25-30C. Cooled the reaction mixture to 0-5C and stirred for 60 mins at the same temperature.Filtered the precipitated solid, washed with water and dried to get the title compound.Yield: 46 gms; Melting range: 172-176C; purity: 96.89%

The chemical industry reduces the impact on the environment during synthesis 2-(Methoxy(4-phenoxyphenyl)methylene)malononitrile. I believe this compound will play a more active role in future production and life.

Reference:
Patent; MSN LABORATORIES PRIVATE LIMITED; THIRUMALAI RAJAN, Srinivasan; ESWARAIAH, Sajja; MADHUSUDHAN, Gutta; SEETHA RAMA SARMA, Peri; (69 pag.)WO2016/170545; (2016); 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. 499983-13-0, name is 4-Bromo-3-fluorophenylacetonitrile belongs to nitriles-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below. Recommanded Product: 499983-13-0

EXAMPLE 3Preparation of ethyl 3-fluoro-4-bromo-phenylacetate from 3-fluoro-4-bromo-phenylacetonitrile2.5 g of 3-fluoro-4-bromo-phenylacetonitrile, 4.7 g. of ethyl alcohol and 4.7 g of sulfuric acid were loaded at room temperature in an reactor. The mixture was heated to 100 C and stirred for 5 hours. When the conversion was completed, the mixture was cooled to room temperature, water and ethyl acetate were added and the aqueous phase was re-extracted with fresh ethyl acetate. The organic phase was washed with a sodium bicarbonate/water solution, then with water until pH=7. The organic phase was concentrated to yield 2.6 g, of crude product.

The synthetic route of 499983-13-0 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; CHIESI FARMACEUTICI S.p.A; VERZINI, Massimo; Cotarca, Livius; Guidi, Alberto; Melloni, Alfonso; Maragni, Paolo; US2014/378696; (2014); A1;,
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Reference of 179898-34-1, A common heterocyclic compound, 179898-34-1, name is 3-Bromo-5-fluorobenzonitrile, molecular formula is C7H3BrFN, 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.

Example 18 1,1-Dimethylethyl [(3-bromo-5-fluorophenyl)methyl]carbamate NaBH4 (1.99 g, 52.5 mmol) was cautiously added to a solution of NiCl2 (1.36 g, 10.5 mmol), Boc2O (4.58 g, 21.0 mmol) and 3-bromo-5-fluorobenzonitrile (2.10 g, 10.5 mmol) in absolute ethanol (30 mL) at 0 C. (vigorous reaction with the formation of a black precipitate). Once the reaction had subsided the mixture was left to stir at room temperature for 30 min. Ethanol was removed under reduced pressure and the precipitate was dissolved in EtOAc, filtered and repeatedly washed with EtOAc. The combined organic phase was washed with saturated NaHCO3, and dried over Na2SO4. After removing the solvent, the product was purified by flash column chromatography to yield 1,1-dimethylethyl [(3-bromo-5-fluorophenyl)methyl]carbamate (2.20 g, 69%). 1H NMR (400 MHz, CDCl3): delta 1.46 (S, 9H), 4.28-4.32 (m, 2H), 4.87 (br, 1H), 6.93-7.29 (m, 3H); 13C NMR (100 MHz, CDCl3): delta 20.3, 43.6, 44.1, 79.7, 80.0, 113.0, 114.0, 117.7, 122.5, 126.0, 123.0, 141.7, 155.9, 161.5, 164.0.

The synthetic route of 179898-34-1 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Glaxo Group Limited; US2009/197871; (2009); A1;,
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These common heterocyclic compound, 51632-29-2, name is 2-(3-Phenoxyphenyl)acetonitrile, 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. Formula: C14H11NO

1.38 g (6.59 mmol) of 3-phenoxyphenylacetonitrile and 1.57 g (6.59 mmol) of cobalt(II) chloride hexahydrate are dissolved in 25 ml of methanol. The solution is cooled with an iced water bath and 1.74 g (46 mmol) of sodium borohydride are added in portions. The reaction mixture is stirred overnight at ambient temperature. It is filtered on paper and rinsed with twice 25 ml of methanol. The filtrate is concentrated under reduced pressure and the residue is taken up in 50 ml of aqueous hydrochloric acid (1N) and 25 ml of ether. After distinct phases have separated out they are separated. The aqueous phase is washed with three times 25 ml of ether. The aqueous phase is rendered alkaline with 10 ml of aqueous 36% sodium hydroxide and extracted with three times 50 ml of dichloromethane. The extracts are washed with saturated aqueous sodium chloride solution and dried over sodium sulphate and the filtrate is concentrated under reduced pressure. This gives 0.67 g of product in the form of a brown-orange oil, which is used as it is in the following step

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

Reference:
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Adding a certain compound to certain chemical reactions, such as: 97165-77-0, name is 3,5-Dibromobenzonitrile, 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 97165-77-0, Quality Control of 3,5-Dibromobenzonitrile

3,5-dibromobenzene cyanide (20.0 mmol) under nitrogen protection,1-THP-4-pyrazoleboronic acid pinacol ester (48.0 mmol) and 1,4-dioxane (120 mL) and water (30 mL) were added to a 250 mL round bottom flask.Add magnetron stirring, then add K2CO3 (60.0mmol)And Pd(PPh3)4 (1.0 mmol), the reaction was stirred at 100 C for 24 hours. After the reaction is completed, the solvent of the reaction system is spin-dried.The residue was dissolved in ethyl acetate (200 mL).Wash with water (150 mL × 2) and saturated brine (200 mL),After drying over anhydrous Na 2 SO 4 , filtered and concentrated.The crude product was purified by column chromatography (SiO2, petroleum ether / ethyl acetate = 20:1 to 1:1).After concentration, 3,5-bis(1-(tetrahydro-2H-pyran-2-yl)-1H-pyrazol-4-yl)phenyl cyanide was obtained as a pale yellow solid (yield: 84%).

If you are interested in these compounds, you can also browse my other articles.Thank you for taking the time to read this article. I hope you enjoyed it.

Reference:
Patent; Beijing University of Technology; Li Jianrong; Kong Xiangjing; Zhang Yongzheng; He Tao; (10 pag.)CN109851559; (2019); A;,
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Reference of 1735-53-1, 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. 1735-53-1, name is 4-Bromo-3-(trifluoromethyl)benzonitrile belongs to nitriles-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

A mixture of [4-BROMO-3- (TRIFLUOROMETHYL)-BENZONITRILE] (Yonezawa [ET AG,] Synthetic Communications (1996) 26,1575-8 ; 2.47 g, 12 [MMOL),] 1-methylpiperazine (Fluka, Buchs, Switzerland, 5.33 mL, 48 [MMOL)] and 15 mL [N, N-DIMETHYLACETAMIDE] is stirred in a tightly closed vessel for 14 hours at [95C.] After cooling, the reaction mixture is evaporated to dryness under reduced pressure and the residue is treated with a half-saturated aqueous solution of sodium carbonate and extracted with ethyl acetate. The combined extracts are dried [(NA2SO4)] and the solvent is evaporated off under reduced pressure. The crude product is purified by column chromatography on silica gel, eluent methylene chloride/methanol to give [4- (4-METHYL-1-PIPERAZINYL)-3- (TRIFLUOROMETHYL)-BENZONITRILE] as a pale yellow oil. A mixture consisting of 30 mL dioxane, 15 mL water and 11.25 mL of 2M aqueous sodium hydroxide solution is added to [4- (4-METHYL-1-PIPERAZINYL)-3- (TRIFLUOROMETHYL)-BENZONITRILE] and the reaction mixture is shaken for 16 hours at [95C.] After cooling, the mixture is evaporated. The resulting residue is treated with water, the pH adjusted [TO-5-6] with 1 M hydrochloric acid and the solvent evaporated off under reduced pressure. The residue is treated with hot methanol, the insoluble salt filtered off and the filtrate evaporated yielding the crude title compound which is used for the next step without further purification. [‘H-NMR] (400 MHz, [DMSO-D6,] [8)] : 2.28 (s, 3H); 2.50-2. 58 (m, 4H); 2.94-3. 02 (m, 4H); 7.52 [(M, 1 H) ; 8.11-8. 17 (M, 2H); 13.19 (BR. , 1 H).]

The synthetic route of 4-Bromo-3-(trifluoromethyl)benzonitrile has been constantly updated, and we look forward to future research findings.

Reference:
Patent; NOVARTIS AG; NOVARTIS PHARMA GMBH; WO2004/29038; (2004); A1;,
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Adding a certain compound to certain chemical reactions, such as: 62088-13-5, name is Ethyl 3-(3-cyanophenyl)-3-oxopropanoate, 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 62088-13-5, Application In Synthesis of Ethyl 3-(3-cyanophenyl)-3-oxopropanoate

Example K9 {2-[3-(3-Cyano-phenyl)-3-oxo-propionylamino]-4-furan-3-yl-phenyl}-carbamic Acid tert.-Butyl Ester Prepared from (2-amino-4-furan-3-yl-phenyl)-carbamic acid tert.-butyl ester (Example G11) and 3-(3-cyano-phenyl)-3-oxo-propionic acid ethyl ester (Pol. J. Chem. 1978, 25) according to the general procedure K. Obtained as an orange solid (460 mg). MS (ISP) 446 [(M+H)+], 463 [(M+NH4)+] and 468 [(M+Na)+]

If you are interested in these compounds, you can also browse my other articles.Thank you for taking the time to read this article. I hope you enjoyed it.

Reference:
Patent; Hoffmann-La Roche Inc.; US6509328; (2003); B1;,
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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. 36282-26-5, name is 2-Bromo-4-fluorobenzonitrile, A new synthetic method of this compound is introduced below., Product Details of 36282-26-5

Example 4; 3-bromo-4-cyanophenylhydrazine; In a clean, dry 250-mL round-bottom flask, 2-bromo-4-fluorobenzonitrile (25.34 g) was dissolved in tetrahydrofuran (50 mL) under N2. To this was slowly added anhydrous hydrazine (50 mL). The solution color changed from yellow to red-orange. The reaction was allowed to stir at room temperature for 16 hours. A yellow-white crystalline solid precipitated from the solution. The mixture was then diluted with THF (50 mL) to dissolve the solids. The organic layer was then washed with saturated sodium bicarbonate solution until the pH of the organic layer was approximately 8.5. The organic layer was isolated and the solvent was removed under reduced pressure to give a white solid. This was place in a fritted glass funnel and washed with 1.5 L of water, followed by of diethyl ether (ca. 200 mL). The ether wash was then combined with the white solid and dried under reduced pressure. The title compound was isolated as a fluffy, white or off-white solid (23.43 g, 87.20% yield). MS m/z: calculated=212.05; m/z observed=252.98 (M+41).

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; Huang, Kenneth He; Eaves, Jeron; Veal, James; Hall, Steven E.; Barta, Thomas E.; Hanson, Gunnar J.; US2007/207984; (2007); A1;,
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