Month: May 2021

Reference of 110-67-8, 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. 110-67-8, name is 3-Methoxypropanenitrile belongs to nitriles-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

methyl cyanoacetate9 bar of O2 were injected into a solution of 3.0 g (0.035 mol) of 3-methoxypropionitrile (Fluka), 0.5 g (3.0 mmol) of NHPI (N-hydroxy-phthalimide) and 57 mg (0.23mmol) of Co(CH3COO)2.4H2O in 50 ml of acetic acid in a pressure autoclave. The mixture was subsequently stirred at 150 C. for 5 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-Methoxypropanenitrile, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; Lonza AG; US6700010; (2004); B1;,
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Adding a certain compound to certain chemical reactions, such as: 362527-61-5, name is Ethyl 3-bromo-4-cyanobenzoate, 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 362527-61-5, Recommanded Product: 362527-61-5

EXAMPLE 206A 3-bromo-4-cyanobenzoic acid A solution of Example 87C (150 mg) in methanol (3 mL) and water (1 mL) was treated with LiOH (80 mg) and stirred for 2 hours. The solution was adjusted to pH 2 with 1M HCl, then extracted with ethyl acetate. The extract was dried (MgSO4), filtered, and concentrated to provide the desired product of sufficient purity for subsequent use without further purification. MS (DCI/NH3) m/z 243 and 245 (M+NH4)+; 1H NMR (300 MHz, CDCl3) delta 8.40 (d, 1H), 8.13 (dd, 1H), 7.79 (d, 1H).

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; Wang, Wei-Bo; Curtin, Michael L.; Fakhoury, Stephen A.; Gwaltney II, Stephen L.; Hasvold, Lisa A.; Hutchins, Charles W.; Li, Qun; Lin, Nan-Horng; Nelson, Lissa Taka Jennings; O’Connor, Steve; Sham, Hing L.; Sullivan, Gerard M.; Wang, Gary T.; Wang, Xilu; US2002/19527; (2002); A1;,
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Synthetic Route of 3100-67-2, A common heterocyclic compound, 3100-67-2, name is 1-Amino-2-naphthonitrile, molecular formula is C11H8N2, 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.

The dried 1 L reactor was charged with nitrogen and then 50.0 g (297 mmol) of intermediate 13-a,500 mL of dimethylformamide is stirred.55.56 g (312 mmol) of N-bromosuccinimide are slowly added to the reactor.Stir at room temperature for 4 hours.When the reaction was completed, distilled water was added dropwise at room temperature to precipitate brown crystals. The crystals were separated by filtration and separated by column chromatography to obtain 68 g of intermediate 13-b.(Yield: 93%)

The synthetic route of 3100-67-2 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; SFC Ltd.; Choi Yeong-tae; Lee Se-jin; Park Seok-bae; Ryu Tae-jeong; Yang Byeong-seon; Lee Da-jeong; (92 pag.)KR2018/10087; (2018); A;,
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Reference of 906673-45-8, A common heterocyclic compound, 906673-45-8, name is 4-(4-Bromo-3-(hydroxymethyl)phenoxy)benzonitrile, molecular formula is C14H10BrNO2, 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.

In a three-necked flask, compound II (1.9 g), tetrahydrofuran (57 mL), triisopropyl borate (1.53 g) were added to cool down to -78C, and butyllithium (6.25 mL, 2.5 M concentration) was added dropwise.After completion of the reaction for 30 minutes or more, after completion of the reaction, 1N hydrochloric acid (57 mL) was added to quench the reaction, stirred for 30 minutes or more, and allowed to stand for stratification.The organic phase was concentrated under reduced pressure until no solvent was evaporated. Methanol (20 mL) was added to the obtained oil, concentrated hydrochloric acid (0.5 mL) was stirred at room temperature overnight, and after completion of the reaction, the mixture was concentrated under reduced pressure to obtain the target compound I (about 1.8 g).

The synthetic route of 906673-45-8 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Yaoyuan Pharmaceutical Chemical (Shanghai) Co., Ltd.; Wang Yuan; Liu Chuanjun; Tang Wensheng; He Xungui; (8 pag.)CN107759625; (2018); A;,
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Related Products of 1897-43-4, These common heterocyclic compound, 1897-43-4, name is 2,5-Dichloroterephthalonitrile, 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.

Under nitrogen atmosphere, 15.4 g of the intermediate (A), 6.64 g of 2,5-dichloroterephthalonitrile, 10.2 g of potassium carbonate, 112 mL of N-methyl-2-pyrrolidinone were put into a flask and stirred at 100 degrees C. for six hours and subsequently at 150 degrees C. for nine hours. After cooled down to the room temperature, the reaction solution was extracted with toluene. After an aqueous layer was removed, an organic layer was washed with a saturated ammonium chloride aqueous solution. After dried with magnesium sulfate, the organic layer was concentrated. The obtained residue was refined by silica-gel column chromatography, whereby 5.27 g (yield 28%) of a yellow solid of a compound 1 was obtained. It should be noted that N-methyl-2-pyrrolidinone is occasionally abbreviated as NMP.

Statistics shows that 2,5-Dichloroterephthalonitrile is playing an increasingly important role. we look forward to future research findings about 1897-43-4.

Reference:
Patent; Idemitsu Kosan Co., Ltd.; TASAKI, Satomi; KAWAMURA, Masahiro; OGIWARA, Toshinari; KUMA, Hitoshi; YOSHIDA, Kei; OKINAKA, Keiji; (240 pag.)US2016/130225; (2016); A1;,
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Electric Literature of 394-47-8, 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. 394-47-8, name is 2-Fluorobenzonitrile belongs to nitriles-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

To a solution of compound B1 (5.00 g, 41.3 mmol) and phenol (5.80 g, 61.9 mmol) in DMA (50 mL) was added l8-crown-6 (1.10 g, 4.13 mmol) and K2C03 (11.4 g, 82.6 mmol), the reaction mixture was stirred at H0C for 16 hours to give a brown mixture. LCMS showed the reaction was complete. To the reaction mixture was added H20 (50 mL), the reaction mixture was extracted with EtOAc (50 mL x 3), the combined organic phase was washed with H20 (40 mL x 2) and brine (100 mL), dried over anhydrous Na2S04, filtered and concentrated under reduced pressure to give a brown oil, which was purified by Combi Flash to give compound B2 (9.80 g) as a yellow 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, 2-Fluorobenzonitrile, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; QURIENT CO., LTD.; LEAD DISCOVERY CENTER GMBH; NAM, Kiyean; KIM, Jaeseung; JEON, Yeejin; YU, Donghoon; SEO, Mooyoung; PARK, Dongsik; EICKHOFF, Jan; ZISCHINSKY, Gunther; (217 pag.)WO2019/197549; (2019); A1;,
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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. 64113-86-6, name is 5-Methyl-2-nitrobenzonitrile, A new synthetic method of this compound is introduced below., Recommanded Product: 5-Methyl-2-nitrobenzonitrile

In a 1.0 L round bottomed flask, 12.375 g of the above nitrile and 12.30 grams of methyl-4-formylbenzoate were dissolved in 500 mL MeOH and 20.25 mL NaOMe was added. The reaction is allowed to stir for 96 hours, acidified with TFA to pH 4.0, chilled for 1 hour, filtered and washed with MeOH. Yield, 7.0 g; mp 266-269 C.; MS (FAB), (C17 H12 N2 O4), calcd, 308; found 309 (MH+).

The synthetic route of 64113-86-6 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Nair, Madhavan G.; US2010/260825; (2010); A1;,
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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. 362527-61-5, name is Ethyl 3-bromo-4-cyanobenzoate, A new synthetic method of this compound is introduced below., HPLC of Formula: C10H8BrNO2

STEP 1 : To a pressure vessel were added ethyl 3-bromo-4-cyanobenzoate (500 mg, 1.97 mmol), cesium carbonate (1.28 g, 3.94 mmol), pentan-3 -amine (688 uL, 5.90 mmol), XANTPHOS (1 14 mg, 0.20 mmol), tris(dibenzylideneacetone)dipalladium(0) (90 mg, 0.10 mmol), and dioxane (3 mL). The vessel was sealed and heated to 95 C for 15 h. After cooling to room temperature, the mixture was filtered through celite and the filter cake rinsed with ethyl acetate. The filtrate was then concentrated and the residue was purified by column chromatography (10% ethyl acetate in hexanes) to provide ethyl 4-cyano-3- (pentan-3-ylamino)benzoate (315 mg, 1.21 mmol, 61% yield) as a yellow syrup. 1H NMR (400 MHz, CDCl3): 7.43 (d, IH), 7.33 (s, I H), 7.25 (dd, IH), 4.44-4.35 (m, 3H), 3.48-3.40 (m ,1H), 1..72-1.48 (m ,4H), 1.40 (t, 3H), 0.96 (t, 6H); MS (EI) for Ci5H20N2O2: 261 (MH+).

The synthetic route of 362527-61-5 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; EXELIXIS, INC.; WO2009/55077; (2009); A1;,
Nitrile – Wikipedia,
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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. 13989-82-7, name is 4-(Dimethylamino)butanenitrile, A new synthetic method of this compound is introduced below., Safety of 4-(Dimethylamino)butanenitrile

To a suspension of lithium aluminum hydride (LAH) (4.74 g, 120.90 mmol) in dry ether (100 ml) was added dropwise a solution of N-(3-cyanopropyl)-N,N-dimethylamine 321 (4.10 g, 36.61 mmol) in dry ether (50 ml) at 0 C. After complete addition, the reaction mixture was stirred for two hours while allowing the temperature to raise from 0 C. to room temperature. The reaction mixture was quenched with 2N NaOH at 0 C., and the resulting white suspension was filtered through Celite and washed with ether. The ether filtrate was dried over K2 CO3, filtered and concentrated in vacuo, yielding N,N-dimethyl-1,4-diaminobutane 322 as a colorless oil (2.5 g, 60% yield). 1 H NMR (400 MHz, CDCl3) delta: 1.43 (4H, m, –CH2 –CH2 –CH2 –CH2 –), 1.93 (2H, br s, –NH2), 2.16 (6H, s, –N(CH3)2), 2.21 (2H, t, –CH2 CH2 N), 2.66 (2H, t, –CH2 CH2 NH2).

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; Magainin Pharmaceuticals Inc.; US5721226; (1998); A;,
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Reference of 55984-93-5,Some common heterocyclic compound, 55984-93-5, name is 2-Methylterephthalonitrile, molecular formula is C9H6N2, 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.

General procedure: A 10?mL Pyrex tube equipped with a magnetic stir bar wascharged with 1,4?DCB (25.6 mg, 0.2 mmol), fac?Ir(ppy)3 (2.6mg, 2 molpercent) and DMSO (2 mL). The Pyrex tube was sealed with rubber plug and then deaerated by bubbling Ar for 15 min, then benzaldehyde (30.5 muL, 0.3 mmol) and DIPEA (52.4 muL, 0.3mmol) were added. The reaction system was irradiated with blue LEDs (lambda = 450 ± 10 nm) for 12 h at RT. When the reaction was complete, the aqueous solution was extracted with ethyl acetate (5 mL × 3). The organic extracts were combined, washed with brine and dried over anhydrous sodium sulfate.The solvent was removed under vacuum and the residue was purified by chromatography on silica gel (petroleum ether:ethyl acetate = 3:1) to afford the desired product.

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 2-Methylterephthalonitrile, its application will become more common.

Reference:
Article; Liu, Zan; Nan, Xiaolei; Lei, Tao; Zhou, Chao; Wang, Yang; Liu, Wenqiang; Chen, Bin; Tung, Chenho; Wu, Lizhu; Cuihua Xuebao/Chinese Journal of Catalysis; vol. 39; 3; (2018); p. 487 – 494;,
Nitrile – Wikipedia,
Nitriles – Chemistry LibreTexts