Month: August 2021

Related Products of 685-88-1, These common heterocyclic compound, 685-88-1, name is Diethyl fluoromalonate, 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.

Step 2: Preparation of Compound a4 (0634) (0635) To a solution of Compound a2 hydrochloride (1.0 g, 5.25 mmol) in methanol (10 mL) was added potassium tert-butoxide (1.07 g, 9.54 mmol), the mixture was stirred 10 minutes under ice-cooling. After added Compound a3 (739 ul, 4.77 mmol), the solution was stirred at 60 C. for 1 hour. After added 2 mol/L hydrochloric acid aqueous solution, methanol was removed under reduced pressure. The precipitated solid was filtered, washed with water, and concentrated under reduced pressure to yield Compound a4 (648.8 mg, yield: 57%) as pale pink solid. (0636) LC-MS: m/z=241. [M+H]+ (0637) LC/MS method: Method A, retention time: 0.74 min

Statistics shows that Diethyl fluoromalonate is playing an increasingly important role. we look forward to future research findings about 685-88-1.

Reference:
Patent; The University of Tokyo; TOHOKU UNIVERSITY; Shionogi & Co., Ltd.; NAGANO, Tetsuo; OKABE, Takayoshi; KOJIMA, Hirotatsu; KAWAGUCHI, Mitsuyasu; NUREKI, Osamu; ISHITANI, Ryuichiro; NISHIMASU, Hiroshi; AOKI, Junken; TANAKA, Nobuyuki; KANDA, Yasuhiko; KIOI, Yoshiyuki; TATENO, Yusuke; KIDA, Shiro; YAMANE, Junji; (163 pag.)US2017/158704; (2017); A1;,
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Electric Literature of 14062-18-1, 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 14062-18-1 as follows.

Reference Example 46; Ethyl alpha- (hydroxymethylene)-4-methoxyphenyl acetate Sodium hydride (60% in oil) (467 mg, 11.7 mmol) was added to a benzene solution (10 ml) of ethyl 4-methoxyphenyl acetate (2.0 g, 10.3 mmol), while being cooled with ice. The mixture was stirred at room temperature for 5 minutes. The stirred mixture was cooled with ice again; ethyl formate (1.02 ml, 12.6 mmol) was added thereto, and stirred at room temperature for 3 hours. While being cooled with ice, water and ethyl acetate were added to the reaction mixture, and then 2N hydrochloric acid (6 ml) was added to separate the reaction mixture into two layers. The organic layer was concentrated under reduced pressure, and the residue was then purified by silica gel column chromatography (n-hexane : ethyl acetate = 4 : 1). The purified product was concentrated under reduced pressure to thereby obtain 1.97 g of oily slightly reddish-brown ethyl alpha- (hydroxymethylene) -4- methoxyphenyl acetate (yield: 86%) . The resultant compound undergoes nitrogen substitution, and was stored in a freezer. 1H-NMR (CDCl3) dppm:1.28 (3H, t, J=7.1 Hz), 3.81 (3H, s), 4.28 (2H, q, J=7.1 Hz), 6.87 (2H, d, J=8.8 Hz), 7.16-7.26 (3H, m) , 12.02 (IH, d, J=12.5 Hz)

According to the analysis of related databases, 14062-18-1, the application of this compound in the production field has become more and more popular.

Reference:
Patent; OTSUKA PHARMACEUTICAL CO., LTD.; WO2008/150029; (2008); A1;,
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Related Products of 40872-87-5, A common heterocyclic compound, 40872-87-5, name is Methyl 3-amino-4-chlorobenzoate, molecular formula is C8H8ClNO2, 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.

7-Oxo-7,8-dihydropyrido[2,3-d]pyrimidine-6-carboxylic acid (0.275 g, 1.44 mmol) and methyl 3-amino-4-chlorobenzoate (401 mg, 2.16 mmol) was suspended in DMF (4.5 mL). Triethylamine (728 mg, 7.19 mmol) was added, resulting in a clear, pale yellow solution. HATU (821 mg, 2.16 mmol) was then added. Solid began to precipitate out of solution again after 30 minutes. After stirring at room temperature for 6 hours the thick mixture was diluted with EtOAc. The solid was collected and dried to give methyl 4-chloro-3-(7-oxo-7,8-dihydropyrido[2,3-d]pyrimidine-6-carboxamido)benzoate. (Yield 0.295 g, 822 mumol, 57.2%).

The synthetic route of 40872-87-5 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Anderson, Kevin; Chen, Yi; Chen, Zhi; Luk, Kin-Chun; Rossman, Pamela Loreen; Sun, Hongmao; Wovkulich, Peter Michael; US2012/184542; (2012); 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. 150726-89-9, name is Dimethyl 2-(2-methoxyphenoxy)malonate, This compound has unique chemical properties. The synthetic route is as follows., name: Dimethyl 2-(2-methoxyphenoxy)malonate

a) At 5 C. 12.7 g of sodium methylate was added portionwise to a solution of 18.9 g of dimethyl-2-(o-methoxyphenoxy)malonate in 450 ml of methanol. Upon completion of the addition stirring was continued at room temperature for 30 min followed by the addition of 6 g of formamidine hydrochloride. The mixture was stirred at room temperature for 72 h. Eventually, the solvent was removed under reduced pressure and the remaining residue was suspended in diethyl ether. The solid material was filtered off and dissolved in 100 ml of water. The solution was acidified with conc. hydrochloric acid. A white precipitate formed. The precipitate was collected, washed with water and dried to give 15.1 g of 5-(o-methoxyphenoxy)-4,6-dihydroxy-pyrimidine (or a tautomer) as a white powder.

According to the analysis of related databases, 150726-89-9, the application of this compound in the production field has become more and more popular.

Reference:
Patent; Actelio Pharmaceuticals Ltd.; US6596719; (2003); B1;,
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Electric Literature of 39149-80-9, A common heterocyclic compound, 39149-80-9, name is tert-Butyl 2-bromopropanoate, molecular formula is C7H13BrO2, 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.

To a stirred solution 9.5 g (0.10 mol) of 2-hydroxypyridine in 250 mL of DMF was added 16.6 g (0.120 mol) of potassium carbonate followed by 25.0 g (0.120 mol) of 2- bromopropionic acid fert-butyl ester. The resulting mixture was stirred at ambient temperature for 7 h then diluted with IL of water. The aqueous phase was extracted with ethyl acetate (3 x 200 mL) and the combined organics were washed with water (2 x 100 mL), brine (100 mL), dried over magnesium sulfate, filtered and evaporated in vacuo. The crude residue was purified by silica gel chromatography eluting with 25% ethyl acetate in hexanes to afford the title compound as a clear gum 16 g (72%). LC-MS: m/z (ES) 224 (MH)+

The synthetic route of 39149-80-9 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; MERCK & CO., INC.; WO2009/123870; (2009); A1;,
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Adding a certain compound to certain chemical reactions, such as: 5445-17-0, name is Methyl 2-bromopropanoate, belongs to esters-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 5445-17-0, Formula: C4H7BrO2

General procedure: An appropriate diphenyl diselenide (2.96g, 9.5 mmol) was dissolved in a 1:1 mixture of water and THF (50 mL) under nitrogen gas. NaBH4 (1.79g, 47.5 mmol) was added. The reaction mixture was stirred until the solution turned colorless (1-3 minutes). The reaction mixture was stirred for a further 30 minutes. A solution of a methyl -2-bromoacetate (2.96g, 19.37 mmol) in THF (5 mL) was added through the rubber septum without opening the reaction apparatus. The reaction mixture was stirred at room temperature and monitored via TLC (~4 hours). Subsequently, the solution was stirred for a further 30 minutes on air, then the reaction mixture was diluted with 50 mL of saturated aqueous solution of NH4Cl and extracted with diethyl ether. The combined organic phases were dried over Na2SO4, filtered and the solvent was evaporated under reduced pressure to get the product.

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

Reference:
Article; Ali, Wesam; Wi?cek, Ma?gorzata; ?a?ewska, Dorota; Kurczab, Rafa?; Jastrz?bska-Wi?sek, Magdalena; Sata?a, Grzegorz; Kucwaj-Brysz, Katarzyna; Lubelska, Annamaria; G?uch-Lutwin, Monika; Mordyl, Barbara; Siwek, Agata; Nasim, Muhammad Jawad; Partyka, Anna; Sudo?, Sylwia; Latacz, Gniewomir; Weso?owska, Anna; Kie?-Kononowicz, Katarzyna; Handzlik, Jadwiga; European Journal of Medicinal Chemistry; vol. 178; (2019); p. 740 – 751;,
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Adding a certain compound to certain chemical reactions, such as: 61644-18-6, name is Chloromethyl isobutyrate, belongs to esters-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 61644-18-6, Product Details of 61644-18-6

In a reactor equipped with a distillation device, add toluene,100 g (0.55 mol) of ethyl 1-ethyl-3-methylpyrazole-5-carboxylate and 95 g (0.55 mol) of p-tert-butylbenzoacetonitrile, after dehydration under reflux,224g (0.66mol) of sodium ethoxide solution was added dropwise, and the addition was completed within 5h.Low-boiling by-products are separated from the top of the column.After the reaction was completed, the solvent and other boilables were distilled off under reduced pressure, and toluene was recovered.To the residue were added anhydrous acetonitrile and 4.5 g (0.03 mol) of sodium iodide.Add 77.8g (0.57mol) of 1-chloromethyl isobutyrate,Warm to reflux.After the reaction is completed, cool and separate the liquid phase.The solvent was distilled off under reduced pressure,Get 213.7g1- (2- (4- (tert-butyl) phenyl) -2-cyano-1- (1-ethyl-3-methyl-1H-5-pyrazolyl) ethoxy) isobutyric acid Methyl ester,The yield was 95%, in which the content of the E formula was 88.4%.

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, Chloromethyl isobutyrate, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; Zhejiang Chemical Institute Co., Ltd.; Sinochem Lantian Group Co., Ltd.; Zhong Liangkun; Xu Tianming; Huang Hongying; Wei Youchang; (16 pag.)CN110003111; (2019); A;,
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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. 75567-84-9, name is Methyl 3-(4-bromophenyl)propanoate, This compound has unique chemical properties. The synthetic route is as follows., Quality Control of Methyl 3-(4-bromophenyl)propanoate

To a 8 mL sealed tube was added (1S,4S,5R)-5-[[l-cyclopropyl-4-(2,6-dichlorophenyl)- 1H-pyrazol-5-yl]methoxy]-2-azabicyclo[2.2.1]heptane 41g (150 mg, 0.40 mmol, 1.00 equiv.), a solution of methyl 3-(4-bromophenyl)propanoate (116 mg, 0.48 mmol, 1.20 equiv.) in toluene (3 mL), Ru-phos (38 mg, 0.08 mmol, 0.20 equiv.), Ru-phos-precatalyst (68 mg, 0.08 mmol, 0.20 equiv.), and Cs2CO3 (260 mg, 0.80 mmol, 2.00 equiv.). The resulting mixture was heated at 110C overnight. Upon cooling to room temperature, the mixture was diluted with EA (50 mL), washed successively with H2O (50 mL) and brine (50 mL), dried over anhydrous sodium sulfate and concentrated under vacuum. The residue was purified by silica gel column chromatography eluting with ethyl acetate/petroleum ether (1 :3) to give methyl 3-[4-[(1S,4S,5R)-5-[[l- cyclopropyl-4-(2,6-dichlorophenyl)-1H-pyrazol-5-yl]methoxy]-2-azabicyclo[2.2.1]heptan-2- yl]phenyl]propanoate 43a (108 mg, 50%) as a colorless oil.

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 75567-84-9.

Reference:
Patent; ARDELYX, INC.; CHAO, Jianhua; (231 pag.)WO2019/55808; (2019); 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. 927-68-4, name is 2-Bromoethyl acetate belongs to esters-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below. HPLC of Formula: C4H7BrO2

500 mg of the resulting product 6,7-dihydroxy-4- anilinoquinazoline obtained in step 5 of Embodiment 9 was added with 903 mg of 2-bromoethyl acetate, 1.24 g of anhydrous potassium carbonate, 150mg of potassium iodide and 10 ml of dry DMF. The system was reacted overnight at 50C. and followed by TLC until the reaction finished. The reaction solution was diluted with water, extracted with ethyl acetate, washed with saturated sodium chloride solution, dried with anhydrous sodium sulfate and concentrated in vacuum. The crude product was directly put into the next step of reaction without separation.10178] The crude product was dissolved in 20 ml of methanol and then added with 500 mg of KOH. The system was reacted overnight at room temperature and followed by TLC until the reaction finished. The reaction solution was directly concentrated in vacuum and separated by column chromatography to obtain 520 mg of the resulting product 2,2?-(4-(3- ethynylaniline)quinazoline-6,7-diene) di(oxy)diethanol(79%).j0179] ESI mlz 366.0 (M+H)

The synthetic route of 927-68-4 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Guangzhou Institutes of Biomedicine and Health, Chinese Academy of Sciences; Zhang, Yanmei; Ding, Ke; Liao, Jinxi; Wang, Yican; Chen, Panyu; (27 pag.)US2016/175453; (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. 106-65-0, name is Dimethyl succinate, This compound has unique chemical properties. The synthetic route is as follows., name: Dimethyl succinate

Tert-amylalcohol (50 mL), sodium (1.00 g, 43.50 mmol), and catalytic amount of ferricchloride (5 mg) were added to a three-neck round-bottom flask. The mixture washeated at 145 C under reflux until sodium was completely dissolved.Thiophene-2-carbonitrile (1.40 mL, 15.03 mmol) was added and dimethyl succinate(0,92 mL, 7,03 mmol) was added dropwise during 30 minutes. The reaction mixturewas further heated at 145 C under reflux for 2 hours, cooled to 25 C, whereuponmethanol (40 mL) and hydrochloric acid (5 mL, 35%) were added. The resulting darkred precipitate was filtered off and washed with methanol several times.

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 106-65-0.

Reference:
Article; Podlesny, Jan; Dokladalova, Lenka; Pytela, Oldrich; Urbanec, Adam; Klikar, Milan; Almonasy, Numan; Mikysek, Toma?; Jedryka, Jaroslav; Kityk, Iwan V.; Bure?, Filip; Beilstein Journal of Organic Chemistry; vol. 13; (2017); p. 2374 – 2384;,
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