Month: March 2021

Adding a certain compound to certain chemical reactions, such as: 17823-40-4, name is 4-Bromo-2,3,5,6-tetrafluorobenzonitrile, 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 17823-40-4, Recommanded Product: 17823-40-4

A mixture of (1,2-dihydroacenaphthylen-5-yl)boronic acid (1.6 g, 8 mmol), 4-bromo-2,3,5,6-tetrafluorobenzonitrile (1.0 g, 3.9 mmol), Pd2(dba)3 (0.18 g, 0.20mmol), SPhos (0.16 g, 0.4 mmol), K3PO4 (2.0 g, 8.7 mmol) in toluene (50 mL) was degassed and heated at about 120 C for about 16 hours. After filtered off precipitate and washed with toluene, the filtrate was purified by flash column using eluents of hexane to hexane/dichloromethane (7:3). Removal of solvent give awhite solid (Compound 9) (0.54 g, in 42% yield).

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-Bromo-2,3,5,6-tetrafluorobenzonitrile, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; NITTO DENKO CORPORATION; ZHENG, SHIJUN; BASIAGO, ADAM; (86 pag.)JP2016/526025; (2016); A;,
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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. 77-57-6, name is 1-Phenylcyclopentanecarbonitrile, A new synthetic method of this compound is introduced below., Safety of 1-Phenylcyclopentanecarbonitrile

EXAMPLE 16 (R)-1-(2-((((1-Phenylcyclopent-1-yl)methylene)amino)oxy)ethyl)-3-piperidinecarboxylic acid hydrochloride To a solution of 1-phenyl-1-cyclopentanecarbonitrile (7.0 g, 41 mmol) in n-heptane (100 ml) cooled to -30 C. was dropwise added a 1M solution of diisobutylaluminium hydride in n-heptane (82 ml, 82 mmol). The mixture was stirred at -30 C. for 1 h and at 0 C. for 1 h. The mixture was diluted with diethylether (100 ml) and silica gel (60 g) was carefully added keeping the temperature below -30 C. The mixture was then allowed to warm to room temperature and then stirred for 20 h. After filtration the filtrate was washed with water (2*100 ml) and dried (MgSO4). The solvent was evaporated in vacuo to give 3.45 g of the crude 1-phenyl-1-cyclopentanecarboxaldehyde.

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; Novo Nordisk A/S; US5608069; (1997); A;,
Nitrile – Wikipedia,
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Application of 846023-24-3, The chemical industry reduces the impact on the environment during synthesis 846023-24-3, name is 2-Cyano-N-(2,4-dichloro-5-methoxyphenyl)acetamide, I believe this compound will play a more active role in future production and life.

EXAMPLE 44 2-Cyano-N-(2,4-dichloro-5-methoxyphenyl)-3-{4-methoxy-3-[3-(4-methylpiperazin-1-yl)-propoxy]-phenylamino}-acrylamide To a suspension of 2-cyano-N-(2,4-dichloro-5-methoxyphenyl)acetamide (1.75 g, 6.75 mmol) in 8.2 mL of iso-propanol was added triethylorthoformate (1.5 g, 10.1 mmol). The mixture was heated to reflux. After 20 minutes, 4-methoxy-3-[3-(4-methyl-piperazin-1-yl)-propoxy]-phenylamine in 20 mLs of iso-propanol was added dropwise so as to maintain reflux. After 26 hours, the reaction was cooled to room temperature and the suspended solids were filtered. The solids were rinsed with iso-propanol until effluent was colorless. The yellow solid was dried in vacuo to give 3.45 g (93%) of 2-cyano-N-(2,4-dichloro-5-methoxyphenyl)-3-{4-methoxy-3-[3-(4-methylpiperazin-1-yl)-propoxy]-phenylamino}-acrylamide as a mixture of isomers. 1H NMR (300 MHz, CDCl3) delta 11.35 (br d, 1H), 8.17 (m, 2H), 7.76 (d, 1H), 7.41 (s, 1H), 6.88 (m, 1H) 6.69 (m, 2H), 4.10 (t, J=7 Hz, 2H), 3.96 (s, 3H), 3.87 (s, 3), 2.55 (t, J=7 Hz, 2H), 2.48 (m, 8H), 2.29 (s, 3H), 2.06 (m, 2H); MS (ES) m/z548.1 (M+) Analysis for C10H14ClNO2; Calcd: C, 55.69; H, 6.54; N, 6.49. Found: C, 55.49; H, 6.59; N, 6.32.

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, 2-Cyano-N-(2,4-dichloro-5-methoxyphenyl)acetamide, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; Wyeth Holdings Corporation; US2005/43537; (2005); A1;,
Nitrile – Wikipedia,
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Some common heterocyclic compound, 60702-69-4, name is 2-Chloro-4-fluorobenzonitrile, molecular formula is C7H3ClFN, 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: C7H3ClFN

To a solution of 2-chloro-4-fluoro-benzonitrile (4 g, 25.71 mmol) in DMF (20 mL) were added Na2S (3.01 g, 38.57 mmol). The mixture was held at room temperature with stirring on for 20 h. Then the mixture was added 1 M HCl to adjust to pH 6-7. MTBE (20 ml) and water (20 ml) was added. The aqueous phase was extracted with MTBE (20 mL X 2), the combined organic phases were washed with sat. NaHCC”3 (50 mL) and brine (50 mL), dried over anhydrous sodium sulphate. Removal of solvent gave a yellow solid (3.7 g). The residue was used to next step directly. m/z calcd for [C7H4CINS]” [M-H]~: 168.0; found: 168.0.

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 60702-69-4, its application will become more common.

Reference:
Patent; GALECTO BIOTECH AB; BRIMERT, Thomas; JOHNSSON, Richard; LEFFLER, Hakon; NILSSON, Ulf; ZETTERBERG, Fredrik; (284 pag.)WO2016/120403; (2016); A1;,
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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. 75279-53-7, name is 4-Chloro-2-fluorobenzeneacetonitrile, This compound has unique chemical properties. The synthetic route is as follows., HPLC of Formula: C8H5ClFN

To a mixture of 3-chloro-2-fluoro-benzaldehyde (13.7 g, 86.68 mmol, 1.05 eq) and 2- (4-chloro-2-fluoro-phenyl)acetonitrile (14 g, 82.56 mmol, 1 eq) in methanol (200 mL) was added the solution of sodium methoxide (13.4 g, 247.67 mmol, 3 eq) in methanol (40 mL) dropwise at 0 C under nitrogen atmosphere. The product begins to precipitate during the addition. The suspension was stirred at 45 C for 5 hours. The solid was filtered and washed with water (200 mL) and methanol (50 mL) and then was dried in vacuum to give (Z)-3-(3-chloro-2-fluoro- phenyl)-2-(4-chloro-2-fluoro-phenyl)prop-2-enenitrile (24 g, 77.39 mmol, 93% yield) as a white solid. 1H-NMR (400MHz, CDCL) d 8.20 – 8.10 (m, 1H), 7.81 (s, 1H), 7.64 – 7.49 (m, 2H), 7.33 – 7.20 (m, 3H).

According to the analysis of related databases, 75279-53-7, the application of this compound in the production field has become more and more popular.

Reference:
Patent; ARVINAS OPERATIONS, INC.; YALE UNIVERSITY; CREW, Andrew P.; HORNBERGER, Keith R.; WANG, Jing; DONG, Hanqing; BERLIN, Michael; CREWS, Craig M.; (1213 pag.)WO2019/195609; (2019); A2;,
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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. 33279-01-5, name is 3-Oxopentanenitrile, A new synthetic method of this compound is introduced below., Application In Synthesis of 3-Oxopentanenitrile

Step: 1H- thieno[3,2-c] pyrazole-5-carbaldehyde (200mg, 1.314mmol) (see preparation step togetherPreparation Example 1 a) and 3-oxopentanenitrile (191mg, 1.972mmol) wasdissolved in dichloromethane together (20 mL), add The piperidine (11mg,0.131mmol), glacial acetic acid (12mg, 0.197mmol), under nitrogen at refluxovernight trans should. The filtered reaction mixture was cooled to roomtemperature, was added absolute ethanol (20 mL) was diluted reaction mixturewas stirred for ten minutes, filtered It was concentrated to dryness and theresidue was added ethyl acetate (5mL) and petroleum ether (10 mL), stirred forfive minutes and filtered, the solid Dried to give 2 – ((1H- thieno [3,2-c]pyrazol-5-yl) methyl-enyl) -3-oxo-valeronitrile (190mg, 62.5%). ESI-MS: 232 [M+ H].

The synthetic route of 33279-01-5 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Shanghai Huilun life Science & Techonology Co.,Ltd; Cheng, Jianjun; Qin, Jihong; Ye, Bin; (68 pag.)CN103467481; (2016); B;,
Nitrile – Wikipedia,
Nitriles – Chemistry LibreTexts

Reference of 38487-86-4, These common heterocyclic compound, 38487-86-4, name is 2-Amino-4-chlorobenzonitrile, 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.

Add 2-amino-4-chlorobenzonitrile (152 mg, 1 mmol), benzyl alcohol (108 mg, 1 mmol),Fe (NO3) 3 ¡¤ 9H2O (40.4 mg, 0.10 mmol), TEMPO (15.6 mg, 0.10 mmol),t-BuOK (224mg, 2equiv) and 2mL of toluene were sequentially added to a 25mL reaction tube, and the reaction mixture was reacted under reflux for 12h and cooled to room temperature;Ethyl acetate was added to dilute the reaction solution, and then washed three times with water, and then the organic phase was separated.After drying over anhydrous magnesium sulfate, the solvent was removed by rotary evaporation under reduced pressure to obtain a crude product;The crude product was purified by column chromatography with petroleum ether / ethyl acetate, yielding 78%.

The synthetic route of 38487-86-4 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Nanjing University of Science and Technology; Li Bindong; Hu Yongke; (12 pag.)CN110357823; (2019); A;,
Nitrile – Wikipedia,
Nitriles – Chemistry LibreTexts

Synthetic Route of 1835-65-0, A common heterocyclic compound, 1835-65-0, name is 3,4,5,6-Tetrafluorophthalonitrile, molecular formula is C8F4N2, 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.

COMPARATIVE EXAMPLE 2Preparation of a Vanadyl Phthalocyanine CompoundlOg of 3,4,5,6-tetrafluorophthalonitrile, lOg ofthiophenol and 7 g of potassium fluoride were added to 3 neck flask equipped with a reflux apparatus, and then 30 ml of acetonitrile was added as a solvent, and the mixture was reacted withstirring for 12 hours at room temperature. Afier reaction was completed, 7 g of 2,6-dimethylphenol and 4 g of potassium fluoride were added to the reacting solution, and then refluxed for 8 hours. Afier reaction was completed, the solution was distilled with a vacuum distillet 20 g of crude reactantsobtained as above were added to 3 neck flask equipped with a reflux apparatus, and refluxed with 2 g of vanadium trichloride, 2 g of 1-octanol and 30 g of benzonitrile for 8 hours. Afier reaction was completed, the solution was distilled with a vacuum distiller to obtain a vanadyl (vanadium oxide) phthalocyaniene (VOPc: Oxo-Vanadium Phthalocyanine)30 based precursor compound VOPc(PhS)8{2,6-(CH3)2PhO}4F4. 10 g of the vanadyl phthalocyanine-based precursor compound and 50 ml of cyclohexylamine were added to 3 neck flask equipped with a reflux apparatus, and reacted for 8 hours at 60¡ã C. Afier reaction was completed, the reactingsolution was concentrated in vacuum to obtain a vanadyl phthalocyanine compound VOPc(PhS)8{2,6-(CH3)2PhO}4 (C5H11NH)4 (Ph=phenyl; in the formula 2 below, A2, A3, A5, A7, A10, A11, A14 and A15 are PhS; A1, A5, A9 and A13 are {2,6-(CH3)2PhO}; and A4, A8, A12 and A15 are C5H11NH)represented by the formula 2

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; SK CHEMICALS CO., LTD.; Kang, Ju-Sik; Park, Jeong-Ho; Chang, Yu-Mi; US9158048; (2015); B2;,
Nitrile – Wikipedia,
Nitriles – Chemistry LibreTexts

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. 16588-02-6, name is 2-Chloro-5-nitrobenzonitrile, A new synthetic method of this compound is introduced below., Recommanded Product: 16588-02-6

3-Cyano-4-chloroaniline. 2-Chloro-5-nitrobenzonitrile (25 g, 137 mmol) was dissolved in ethanol (275 mL). Stannous chloride dihydrate (154.5 g, 0.685 M) was added and the mixture stirred at 70 C. for 30 min. The mixture was then cooled to room temperature and poured into crushed ice. The mixture was made basic with solid sodium hydroxide. This mixture was extracted with ethyl acetate (3*100 mL). The extracts were combined, washed with brine, dried (MgSO4), concentrated and the residue dried under vacuum and recrystallized from ethanol to yield light brown needles (10.6 g, 51%).

The synthetic route of 16588-02-6 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Chapdelaine, Marc; Davenport, Timothy; Haeberlein, Markus; Horchler, Carey; McCauley, John; Pierson, Edward; Sohn, Daniel; US2004/87575; (2004); A1;,
Nitrile – Wikipedia,
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Related Products of 51762-67-5, 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. 51762-67-5, name is 3-Nitrophthalonitrile belongs to nitriles-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

3-nitrophthalonitrile (20 mmol) and 2,4,6-tris(dimethylaminomethyl)-phenol (20-70 mmol, preferably 60 mmol) as reactants, dimethyl sulfoxide (40) -200 mL, preferably 140 mL, is the solvent, and the reaction is stirred at room temperature ~ 60C (preferably 60C) for 24 to 72 hours in the presence of potassium carbonate (30 to 90 mmol, preferably 80 mmol) and nitrogen, and monitored by thin layer chromatography. Should be filtered to remove the reaction mixture was insoluble potassium carbonate, evaporated to dryness, adding 50 ~ 100mL of chloroform, stirred and filtered to remove insolubles, evaporated to dryness, add 50 ~ 100mL of water to the solid and 15 ~ 45mL HCl (1mol/L) stirred and filtered to remove insolubles. NaOH was added to the filtrate. The solids were precipitated and filtered. The solids were washed with water and dried in vacuo at 50C to give 3-(2,4,6-tris(dimethylamino). Methyl)-phenoxy)phthalonitrile, yield 64%.

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-Nitrophthalonitrile, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; Fuzhou University; Huang Jiandong; Peng Xiaohui; Zheng Bingde; (25 pag.)CN107915740; (2018); A;,
Nitrile – Wikipedia,
Nitriles – Chemistry LibreTexts