Month: March 2021

Reference of 455-68-5, As we all know, there are many different methods for the synthesis of a compound, and people can choose the synthesis method that suits their own laboratory according to the actual situation. 455-68-5 name is Methyl 3-fluorobenzoate, This compound is widely used in many fields, so it is necessary to find a new synthetic route. The downstream synthesis method of this compound is introduced below.

General procedure: A round bottom centrifuge tube containing catalyst 4 (6.7 mol percent based on the percent phosphorus determined by elemental analysis or as otherwise stated in the footnotes of the corresponding Tables) was equipped with a rubber septum and two magnetic stir bars for extra stirring efficiency. After flushing the tube with argon, it was charged via syringe with a higher ester (5 mmol) and MeOH (5 mL) for transesterifications. For amidations, the tube was similarly charged with an ester (2 mmol), amino alcohol (2 mmol), and THF (3 mL). The reaction mixture was vigorously stirred at room temperature (23-25 ¡ãC) and progress of the reaction was monitored by thin layer chromatography. Upon completion of the reaction, the reaction mixture was filtered through Whatman No. 1 filter paper and washed with 3 .x. 10 mL of THF. The combined organics were subjected to short-path silica gel chromatography (0-20percent ethyl acetate in hexanes v/v) to obtain an analytically pure product. In the case of amides, products were purified using a short-path silica gel column eluted with dichloromethane/methanol (95:5, v/v).

At the same time, in my other blogs, there are other synthetic methods of this type of compound, Methyl 3-fluorobenzoate, and friends who are interested can also refer to it.

Reference:
Article; Chintareddy, Venkat Reddy; Ho, Hung-An; Sadow, Aaron D.; Verkade, John G.; Tetrahedron Letters; vol. 52; 49; (2011); p. 6523 – 6529;,
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Synthetic Route of 6962-92-1, 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. 6962-92-1, name is 4-Chlorobutyl acetate belongs to esters-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

Compound 10 (0.40 g, 1.4 mmol) and 4-chlorobutyl acetate (0.25 g, 1.7 mmol) were dissolved in dimethyl acetamide (10 ml). Potassium carbonate (0.24 g, 1.7 mmol) and potassium iodide (47.5 mg, 0.286 mmol) were added to the resulting solution, and then the solution was stirred at 70 C. for 6 hours. After cooling the solution to room temperature, 1 N hydrochloric acid was added to the solution, followed by extraction with ethyl acetate. The organic layer obtained by extraction was washed once with saline, and sodium sulfate was added to the washed organic layer. The obtained organic layer was filtered to collect the filtrate, and then the solvent was distilled off from the filtrate under reduced pressure. The resulting residue was purified by flash column chromatography to obtain Compound 11 (0.49 g) in the form of a pale 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, 4-Chlorobutyl acetate, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; FUJIFILM Corporation; FUKUSHIMA, Yuki; GOTO, Ryoji; US2019/177268; (2019); A1;,
Ester – Wikipedia,
Ester – an overview | ScienceDirect Topics

Electric Literature of 110-38-3, 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. 110-38-3, name is Ethyl caprate, This compound has unique chemical properties. The synthetic route is as follows.

General procedure: In a glove box in a nitrogen atmosphere, 3.33 mg of ruthenium complex 1c (0.005 mmol) Add to a 125-mL Parr autoclave, After adding 11.2 mg of potassium t-butoxide (0.1 mmol), Then take 2mL of tetrahydrofuran and add it to the kettle for a while. Finally, methyl benzoate (1.3615 g, 10 mmol) was added. After the autoclave is sealed, it is taken out of the glove box. Charge hydrogen to 50 atm. The mixture in the reaction kettle was heated and stirred in an oil bath at 120 C for 10 hours, The reactor was cooled to room temperature in a water bath and the remaining gas was slowly drained from the fume hood. Tridecane (50 muL) was added to the mixture as an internal standard, and the yield of methyl benzoate was determined by gas chromatography to be 99%.

The chemical industry reduces the impact on the environment during synthesis Ethyl caprate. I believe this compound will play a more active role in future production and life.

Reference:
Patent; Chinese Academy Of Sciences Shanghai Organic Chemistry Institute; Ding Kuiling; Qiu Jia; Yan Tao; Zhang Lei; Wang Zheng; (49 pag.)CN109553641; (2019); A;,
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Related Products of 94994-25-9, These common heterocyclic compound, 94994-25-9, name is Methyl 4-formylbicyclo[2.2.2]octane-1-carboxylate, 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.

[2-(2-Methyl-1,3-dioxolan-2-yl)ethyl](triphenyl)phosphonium bromide (4-A, Synthesis: 532 (1986)) (5.99 g, 12.7 mmol) was stirred in dry THF (200 mL). Potassium bis(trimethylsilyl)amide (20.4 mL, 2M soln in toluene, 10.2 mmol) was added. The reaction was allowed to stir for 30 min. The reaction mixture was then cooled to -78 C. Methyl 4-formylbicyclo[2.2.2]octane-1-carboxylate was added at -78 C. by cannula. The reaction was allowed to warm to room temperature overnight. The volume was reduced by evaporation of THF in vacuo. 100 mL of water was added. The mixture was then layered with 100 mL of diethyl ether. The ether was extracted and dried (MgSO4). The product (methyl 4-[(1E)-3-(2-methyl-1,3-dioxolan-2-yl)prop-1-enyl]bicyclo[2.2.2]octane-1-carboxylate (4-B)) was purified by flash chromatography on silica gel with 10/90 ethyl acetate-hexane mixture.

The synthetic route of 94994-25-9 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Waddell, Sherman T.; Santorelli, Gina M.; Maletic, Milana M.; Leeman, Aaron H.; Gu, Xin; Graham, Donald W.; Balkovec, James M.; Aster, Susan D.; US2004/133011; (2004); A1;,
Ester – Wikipedia,
Ester – an overview | ScienceDirect Topics

Application of 139102-34-4,Some common heterocyclic compound, 139102-34-4, name is Methyl 4-bromo-2-methoxybenzoate, molecular formula is C9H9BrO3, 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 solution of methyl 4-bromo-2-methoxybenzoate (0.95 g, 3.9 mmol) and 4- nitrophenylboronic acid (1.29 g, 7.75 mmol) in toluene (10 mL) was added Na2CO3 (1.85 g, 17.4 mmol), l,r-bis(diphenylphospMno)ferrocenepalladium(IT) chloride complex with dichloromethane (0.06 g, 0.08 mmol), 1,4-dioxane (5 mL), and water (5 mL). The mixture was heated at reflux for 3 h and then allowed to cool to it. The mixture was diluted with EtOAc and water, and the organic layer was isolated, dried over MgSO4, and concentrated in vacuo. The material was purified by column chromatography (25% EtOAc in hexanes), yielding 0.675 g (61%) of the title compound. LC/MS m/z 287.9 (MH+); retention time 3.14 min.

The synthetic route of 139102-34-4 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; BAYER PHARMACEUTICALS CORPORATION; WO2006/44775; (2006); A2;,
Ester – Wikipedia,
Ester – an overview | ScienceDirect Topics

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. 99974-66-0, name is Diethyl 3-hydroxycyclobutane-1,1-dicarboxylate, A new synthetic method of this compound is introduced below., COA of Formula: C10H16O5

To a solution of compound BB2-C (18 g, 0.0833 mol) in DCM (200 mL) was added PCC (37 g, 0.176 mol) and the mixture was stirred for four hours at room temperature. The solution was filtered through a silica gel column and the residue was washed with DCM/MeOH 98/2 and then filtered through a similar column. The combined fractions were evaporated under reduced pressure to provide the desired compound. TLC system; Petroleum ether: ethyl acetate (9: 1), RF = 0.3. Yield: 1 1 g, 62 %.

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; MEDIVIR UK LIMITED; AYESA, Susana; CARLQUIST, Peter; ERSMARK, Karolina; GRABOWSKA, Urszula; HEWITT, Ellen; JOeNSSON, Daniel; KAHNBERG, Pia; KLASSON, Bjoern; LIND, Peter; ODEN, Lourdes; PARKES, Kevin; WIKTELIUS, Daniel; WO2011/70541; (2011); A1;,
Ester – Wikipedia,
Ester – an overview | ScienceDirect Topics

Related Products of 1014645-87-4, 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. 1014645-87-4, name is Methyl 4-(1-aminocyclopropyl)benzoate hydrochloride belongs to esters-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

The title compound (D171) (58 mg) was prepared according to the experimental procedure described in Description 169 (reaction time 2 h) starting from 5-chloro-2-(3-((4-fluoro-2-methylphenyl)(methyl)amino)azetidin-1-yl)nicotinic acid (D120) (55 mg, 0.157 mmol) and methyl 4-(1-aminocyclopropyl)benzoate (D7) (35.8 mg, 0.157 mmol).

The synthetic route of Methyl 4-(1-aminocyclopropyl)benzoate hydrochloride has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Borriello, Manuela; Rovati, Lucio; Stasi, Luigi Piero; Buzzi, Benedetta; Colace, Fabrizio; US2013/261100; (2013); A1;,
Ester – Wikipedia,
Ester – an overview | ScienceDirect Topics

Electric Literature of 706791-83-5,Some common heterocyclic compound, 706791-83-5, name is Methyl 3-amino-5-bromobenzoate, molecular formula is C8H8BrNO2, 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.

TEA (0.909 ml_, 6.52 mmol) was added to a mixture of propionic acid (0.21 1 ml_, 2.83 mmol) and HATU (1 .157 g, 3.04 mmol) in DMF (1 .0 ml_). After 20 min, methyl 3-amino-5- bromobenzoate (CAS 706791 -83-5) (0.5 g, 2.173 mmol) was added and the resulting mixture was stirred at room temperature for 18 h. The reaction was diluted with EtOAc and water. The aqueous phase was extracted with EtOAc. The combined organic layers were washed with brine, dried over Na2S04, filtered and concentrated. The crude material was purified by flash column chromatography on silica gel (heptane/EtOAc = 100:0 to 0: 100) to give the title compound. 1 H NMR (400 MHz, CHLOROFORM-c/) delta ppm 8.20 (s, 1 H), 7.91 (app. d, J=2.0 Hz, 2 H), 7.15 (br. s. , 1 H), 3.93 (s, 3 H), 2.42 (q, J=7.5 Hz, 2 H), 1 .27 (t, J=7.6 Hz, 3 H).

The synthetic route of 706791-83-5 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; NOVARTIS AG; BELANGER, David B.; FLOHR, Stefanie; GELIN, Christine Fang; JENDZA, Keith; JI, Nan; LIU, Donglei; LORTHIOIS, Edwige Liliane Jeanne; KARKI, Rajeshri Ganesh; MAINOLFI, Nello; POWERS, James J.; RANDL, Stefan Andreas; ROGEL, Olivier; VULPETTI, Anna; YOON, Taeyoung; WO2015/9977; (2015); A1;,
Ester – Wikipedia,
Ester – an overview | ScienceDirect Topics

These common heterocyclic compound, 14273-90-6, name is Methyl 6-bromohexanoate, 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. Recommanded Product: Methyl 6-bromohexanoate

Step-II: Preparation of methyl 6-(3-(benzo[d]oxazol-2-yl)-4-oxoquinolin-l(4H)- yl)hexanoate; To a mixture of 3-(benzo[d]oxazol-2-yl)quinolin-4(lH)-one (0.05 g, 1.9 mmol) and anhydrous K2CO3 (0.078 g, 5.7 mmol) in DMF (5 mL), methyl 6-bromohexanoate(0.079g, 3.8 mmol) was added and heated under microwave at 125 0C for 20 minutes. The reaction mixture was poured into ice-cold water (10 mL) and extracted with ethyl acetate (25 mL). The organic layer was washed with water, brine solution each 10 mL.The organic layer was dried over Na2SO4 and concentrated to afford the crude compound, was purified by column chromatography using 20percent ethyl acetate in hexane as an eluent. The pure fraction was concentrated to afford the title compound as colourless solid (0.055 g, 74.32 percent yield).

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

Reference:
Patent; ORCHID RESEARCH LABORATORIES LTD.; BALASUBRAMANIAN, Gopalan; RAJAGOPAL, Sridharan; RATHINASAMY, Suresh; KILAMBI, Narasimhan; RAJENDRAN, Praveen; NARAYANAN, Shridhar; WO2010/73078; (2010); A2;,
Ester – Wikipedia,
Ester – an overview | ScienceDirect Topics

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. 15848-22-3, name is 5-Bromopentyl acetate, This compound has unique chemical properties. The synthetic route is as follows., Recommanded Product: 15848-22-3

a 5-(3-Bromo-5,5,8,8-tetramethyl-5,6,7,8-tetrahydronaphthalen-2-yloxy)pentyl Acetate A solution of 3-bromo-5,5,8,8-tetramethyl-5,6,7,8-tetrahydronaphthalen-2-ol (10 g, 0.35 mol), 5-bromopentyl acetate (8.15 g) and potassium carbonate (33.6 g) in methyl ethyl ketone (200 ml) is refluxed for 2 hours. The reaction medium is treated with water and ethyl acetate. After separation of the phases by settling, the organic phase is washed twice with water, dried over magnesium sulphate and concentrated on a rotary evaporator under vacuum at 40 C. The product is purified by flash chromatography on a column of silica. Yellow oil. Yield: 93%.

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 15848-22-3.

Reference:
Patent; Galderma Research & Development S.N.C.; US6444709; (2002); B1;,
Ester – Wikipedia,
Ester – an overview | ScienceDirect Topics