Month: July 2021

Electric Literature of 56741-34-5, These common heterocyclic compound, 56741-34-5, name is Methyl 5-amino-2-fluorobenzoate, 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.

General procedure: To a solution of 11a (500 mg, 1.85 mmol) in acetone (10 mL) was added 12 (380 mg, 1.85 mmol) and pyridine (0.45 mL, 5.54 mmol).The mixture was stirred at 55 C for 1 h. The mixture was concentrated,diluted with ethyl acetate and washed with 1M HCl and brine twice.Then, the ethyl acetate layer was dried over anhydrous sodium sulfate andconcentrated to give the crude product. The crude product was purified bysilica column eluting with petroleum ether/ethyl acetate (5/1-2/1) to givethe desired product (0.33 g, yield 44.3%) as grey solid

Statistics shows that Methyl 5-amino-2-fluorobenzoate is playing an increasingly important role. we look forward to future research findings about 56741-34-5.

Reference:
Article; He, Yulong; Dou, Huixia; Gao, Dingding; Wang, Ting; Zhang, Mingming; Wang, Heyao; Li, Yingxia; Bioorganic and Medicinal Chemistry; vol. 27; 19; (2019);,
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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. 10601-80-6, name is Ethyl 3,3-diethoxypropionate belongs to esters-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below. HPLC of Formula: C9H18O4

0463] To a solution of ethyl 3,3-diethoxypropanoate (20 g, 105 mmol) in water (80 ml) was added sodium hydroxide (5 g, 125 mmol, 1.2 eq). The resulting solution was stirred for 1 hour at 110 C. in an oil bath and then adjusted to pH 5 with aqueous hydrogen chloride (3N). The crude product was then extracted with tetrahydrofuran (3×80 ml) and the organic layers were combined, dried over anhydrous sodium sulfate, and filtered before being concentrated under vacuum. The crude residue was purified by silica gel chromatography using 3-50% ethyl acetate in petroleum ether to elute. The product-containing fractions were combined and concentrated under vacuum to afford 3,3-diethoxypropanoic acid as light yellow oil (12 g, 70%); 1H NMR (300 MHz, DMSO): delta 4.80-4.82 (t, J=5.7 Hz, 1H), 3.41-3.61 (m, 4H), 2.49 (d, J=5.7 Hz, 2H), 1.06-1.24 (m, 6H).

The synthetic route of 10601-80-6 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Merial Limited; Meng, Charles Q.; Long, Alan; Huber, Scot; Gurrala, Srinivas Reddy; Wilkinson, Douglas Edward; Pacofsky, Gregory; US2014/142114; (2014); 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. 18014-00-1, name is Dimethyl 2,5-dibromoterephthalate, A new synthetic method of this compound is introduced below., Recommanded Product: 18014-00-1

Carbazole (6.68 g, 0.04 mol),Methyl 2,5-dibromo-1,4-terephthalate (10.48 g, 0.02 mol),O-dichlorobenzene (15ml),Potassium carbonate (5.52 g, 0.04 mol),18-crown-6 (1.07g, 4mmol),Cuprous iodide (0.76g, 4mmol)Mix in a dry single-mouth bottle (50ml),Under the protection of nitrogen atmosphere,Heating to 150 C, stirring and refluxing reaction for 18h ~ 36h,After cooling, suction filtration,Washed with dichloromethane,After rotary evaporation to remove the volatile solvent in the filtrate,Separation by column chromatography,Wet loading,Using petroleum ether/ethyl acetate (6:1) as the eluent,The yellow-green solid product (7.76 g, 14.8 mmol) was obtained.The yield is 74%;

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; Nanjing University of Posts and Telecommunications; Qian Yan; Wang Yingnan; Ye Jingfang; Mi Baoxiu; Gao Zhiqiang; Yi Mingdong; Zhang Guangwei; Xie Linghai; (10 pag.)CN110054581; (2019); 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. 609-08-5, name is Diethyl 2-methylmalonate, A new synthetic method of this compound is introduced below., Formula: C8H14O4

To a THF (0.5 M) solution of diethyl methylmalonate (1 eq.) was added sodium hydride (1.4 eq., 60% (w/w) dispersion in paraffin oil) in four equal portions, three to five minutes apart. The reaction was maintained at 0C for 15 mm, before it was allowed to warm to RT over 30 mm. After another 30 mm of stirring at RT, the mixture was re-cooled to 0C and then added N-fluorobenzenesulfonamide (1.1 eq.) in four equal portions. Stirring was continued at 0C for 30 mm and then at RT for 4 h, at which time it was determined to be >95% complete by ?H NMR. The reaction was then diluted with hexanes and vacuum filtered. The filter cake was washed further with hexanes and the product-containing filtrate was concentrated. More hexanes was added to induce further precipitation of unwanted- by-products and the suspension was filtered again. The filtrate thus obtained was then concentrated in vacuo to furnish a biphasic oil. The upper layer was determined to be paraffin oil and was discarded. The lower layer was the desired product (82% yield).

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; MERCK PATENT GMBH; JORAND-LEBRUN, Catherine; LAN, Ruoxi; CHEN, Austin; CLARK, Ryan C.; (268 pag.)WO2017/49068; (2017); A1;,
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Synthetic Route of 2065-23-8, The chemical industry reduces the impact on the environment during synthesis 2065-23-8, name is Methyl 2-phenoxyacetate, I believe this compound will play a more active role in future production and life.

167.87 g of 99% methyl phenoxyacetate (1 mol), 1.26 g of 99% zinc chloride and 1.68 g of 99% were sequentially added to a 500 mL four-necked flask.2,5-dichlorothiazole, 154.69 g of 99% chlorine (2.16 mol) was introduced at -20 C.After the heat preservation reaction for 30 minutes,Distilling and collecting fractions of 140-150 C under a pressure of 1 kpa,Methyl 2,4-dichlorophenoxyacetate236.21g, content 98.8%,The yield was 99.28% based on methyl phenoxyacetate.

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

Reference:
Patent; Shandong Runbo Biological Technology Co., Ltd.; Sun Guoqing; Hou Yongsheng; Zhang Liguo; Chi Zhilong; Hu Yishan; (12 pag.)CN108947807; (2018); 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. 15224-11-0, name is Ethyl 2-(hydroxymethyl)cyclopropanecarboxylate, A new synthetic method of this compound is introduced below., Quality Control of Ethyl 2-(hydroxymethyl)cyclopropanecarboxylate

EXAMPLE 40 ethyl 2-{[4-chloro-2-({[(5-cyano-2-pyrazinyl)amino]carbonyl}amino)phenoxy]methyl}cyclopropanecarboxylate The desired product (2.5 mg, 6%) was prepared by substituting ethyl 2-(hydroxymethyl)cyclopropanecarboxylate (14.4 mg, 0.10 mmol) for 2-cyclohexen-1-ol in Example 1. MS (ESI(-)) m/z 414 (M-H)-; 1H NMR (500 MHz, DMSO-d6) delta 10.95 (s, 1H), 10.20 (br s, 1H), 8.91 (s, 1H), 8.77 (s, 1H), 8.24-8.28 (m, 1H), 7.04-7.11 (m, 2H), 4.12-4.18 (m, 1H), 3.96-4.08 (m, 3H), 1.82-1.92 (m, 1H), 1.73-1.79 (m, 1H), 1.10-1.19 (m, 4H), 1.02-1.08 (m, 1H).

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; Li, Gaoquan; Li, Qun; Li, Tongmei; Lin, Nan-Horng; Mantei, Robert A.; Sham, Hing L.; Wang, Gary T.; US2004/259885; (2004); A1;,
Ester – Wikipedia,
Ester – an overview | ScienceDirect Topics

Adding a certain compound to certain chemical reactions, such as: 18014-00-1, name is Dimethyl 2,5-dibromoterephthalate, 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 18014-00-1, Recommanded Product: 18014-00-1

A degassed solution of 157.6 g (400 mmol) of diethyl dibromoterephthalate and 36.7 g (220 mmol) of carbazole in 1 l of 1,2-dichlorobenzene is saturated with N2 for 1 h. Then, firstly 20 g (314 mmol) of copper powder, then 18 g (67 mmol) of 18-crown-6 are added to the solution, and 177 g (850 mmol) of potassium carbonate as the solid are subsequently added. The reaction mixture is heated at 170 C. for 18 h. After cooling to room temperature, 1 l of water is carefully added. The organic phase is washed with 4×50 ml of H2O and dried over MgSO4, and the solvents are removed in vacuo. The pure product is obtained by recrystallisation. The yield is 83 g (177 mmol), corresponding to 81% of theory

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; Merck Patent GmbH; Parham, Amir Hossain; Pflumm, Christof; US2013/26422; (2013); A1;,
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Reference of 18014-00-1, 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. 18014-00-1, name is Dimethyl 2,5-dibromoterephthalate belongs to esters-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

2.59 g of compound 2 and 880 mg of 2,5-dibromoterephthalate were dissolved in 100 mL of freshly distilled tolueneMouth,Then, 400 mg of Pd (PPh3) 4 and 330 mg of CuI were added thereto under a nitrogen atmosphere,Heated to reflux for 8-12 hours. After completion of the reaction, the mixture was cooled to room temperature, the reaction solution was poured into water,Extracted with toluene twice, the organic phase was combined, dried, filtered and spin dried to obtain the crude product,The resulting crude product was purified by silica gel column to give 996 mg of compound 3 (84%).

The synthetic route of Dimethyl 2,5-dibromoterephthalate has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Hefei exciton Energy Technology Co., Ltd.; Ding, Jun; (21 pag.)CN106188091; (2016); A;,
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Ester – an overview | ScienceDirect Topics

Electric Literature of 1865-29-8,Some common heterocyclic compound, 1865-29-8, name is Methyl 2-phenylacrylate, molecular formula is C10H10O2, 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 title compound was synthesized according to a literature method (Whitman Tetrahedron 1985, 41, 1183). To a mixture of 2-phenylacrylic acid methyl ester (7.92g, 45 mmol) in 60 ml of methylene chloride was added mCPBA (13. Ig, 58.5 mmol) and the reaction was stirred at 450C overnight. The reaction mixture was then filtered and the solid was washed with methylene chloride. The filtrate was washed three times with 50 ml of equal parts solution consisting of saturated Na2S2O3 and saturated NaHCO3. The organic layer was washed with water and brine, dried over MgSO4, and concentrated under reduced pressure to afford the title compound in greater than 95% purity according to 1H NMR (85% yield). 1H NMR (CDCl3, 300MHz) delta: 7.50 -7.30 (m, 5H), 4.22 (q, J= 7.2 Hz, 2H), 3.40 (d, J, = 7.1 Hz, IH), 2.95 (d, J= 7.1Hz, IH), 1.26 (t, J=7.2Hz, 3H) ppm.

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

Reference:
Patent; YUDIN, Andrei, K.; HILI, Ryan; WO2008/46232; (2008); A1;,
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Ester – an overview | ScienceDirect Topics

Adding a certain compound to certain chemical reactions, such as: 154825-97-5, name is Methyl 2-(4-bromophenyl)-2,2-dimethylacetate, 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 154825-97-5, Application In Synthesis of Methyl 2-(4-bromophenyl)-2,2-dimethylacetate

methyl 3-bromophenyltert-butanoate (formula II) (257g), ethenyl benzyl ether (formula V) (140g), potassium carbonate (138g), and 1,4-dioxane (2L), Replaced 3 times with nitrogen, added tetratriphenylphosphine palladium (3g), and reacted at 100 C for 12h. The reaction was monitored by TLC for completion. The complete reaction system was reduced to room temperature, filtered, and concentrated to remove 1,4-dioxane. Water (1 L) ethyl acetate (1 L) was added, and the layers were separated. The organic phase was dried over anhydrous sodium sulfate and concentrated to dryness to give methyl 4-(2-benzyloxyethenyl)phenyltert-butanoate (formula III) (300 g), yield: 96.7%, purity: 98%.

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

Reference:
Patent; Shanghai Tiancizhong Business Pharmaceutical Co., Ltd.; Chi Wangzhou; Li Hanpu; Ma Xilai; Li Yonggang; Sha Fei; (8 pag.)CN110734375; (2020); A;,
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Ester – an overview | ScienceDirect Topics