Month: January 2021

Synthetic Route of 54535-22-7,Some common heterocyclic compound, 54535-22-7, name is Diethyl 2-((phenylamino)methylene)malonate, molecular formula is C14H17NO4, 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 B: Diethyl N-methyl-N-phenylaminomethylenemalonate To 10 mmol of the compound obtained in the previous Step, dissolved in tetrahydrofuran, there are added, slowly (in small portions) and under an inert atmosphere, 12 mmol of 95% NaH and then, dropwise, 30 mmol of iodomethane. The reaction mixture is then stirred, at ambient temperature and under an inert atmosphere, for 12 hours. 1 mL of methanol is added in order to neutralise the excess of sodium hydride. The solution is then concentrated in vacuo, and then water is added to the residual oil obtained. After extraction with dichloromethane, the combined organic phases are dried, filtered and concentrated under reduced pressure to yield the expected product in the form of a colourless oil. MS (EI, m/z): 276 (M+).

The synthetic route of 54535-22-7 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Brion, Jean-Daniel; Israel, Lucien; Le Ridant, Alain; Harpey, Catherine; Rabhi, Cherif; Kaloun, El Bachir; US2006/63801; (2006); A1;,
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Related Products of 4934-99-0, A common heterocyclic compound, 4934-99-0, name is Methyl 3-hydroxycyclobutanecarboxylate, molecular formula is C6H10O3, 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 N2 atmosphere, a solution of methyl 3-hydroxycyclobutanecarboxylate (7 g, 53.8mmol) in DCM (200 mL) was cooled to -78 oc and DAST (35 mL, 265 mmol, 1.22 g/mL) wasadded. The mixture was stirred at -78 C for 1 h, and the reaction was allowed to warm tort andstirred overnight. The reaction mixture was quenched with H20 (50 mL) at 0 C, and extractedwith DCM (200 mL x 3). The combined organic layers were dried over anhydrous Na2S04, andthen concentrated in vacuo to give the title compound as brown oil (7 g, yield 98.5%). 1HNMR (400 MHz, CDCh) 8 (ppm): 3.70 (s, 3H), 3.58 (q, J= 7.2 Hz, 1H), 3.15-3.10 (m, 1H),2.85-2.76 (m, 1H), 2.54-2.41 (m, 3H);19F NMR (376 MHz, CDCh) 8 (ppm): -151.8.

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; SUNSHINE LAKE PHARMA CO., LTD.; CALITOR SCIENCES, LLC; DAI, Weilong; XI, Ning; LI, Minxiong; ZHANG, Tao; LI, Xiaobo; HU, Haiyang; CHEN, Wuhong; WANG, Tingjin; LIU, Jun; (188 pag.)WO2017/48675; (2017); A1;,
Ester – Wikipedia,
Ester – an overview | ScienceDirect Topics

Electric Literature of 2967-66-0, 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 2967-66-0 as follows.

General procedure: Hydrazine hydrate 64% (v/v) (30.0 mL, 0.33 mol) was heated up to 50-60 C. The methyl ester 3 (0.01 mol) was added and the mixture was heated at reflux for 10 min. The cooling was performed sequentially in water bath, followed by ice bath and dry ice-ethanol bath. The precipitate was filtered and washed with cold water.

According to the analysis of related databases, 2967-66-0, the application of this compound in the production field has become more and more popular.

Reference:
Article; Ishii, Marina; Jorge, Saloma?o Do?ria; De Oliveira, Alex Alfredo; Palace-Berl, Fanny; Sonehara, Ieda Yuriko; Pasqualoto, Kerly Fernanda Mesquita; Tavares, Leoberto Costa; Bioorganic and Medicinal Chemistry; vol. 19; 21; (2011); p. 6292 – 6301;,
Ester – Wikipedia,
Ester – an overview | ScienceDirect Topics

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. 3618-04-0, name is trans-Ethyl 4-hydroxycyclohexanecarboxylate belongs to esters-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below. name: trans-Ethyl 4-hydroxycyclohexanecarboxylate

Step A) Ethyl 4-(tetrahydro-2H-pyran-2-yloxy)cyclohexanecarboxylatePyridinium-4-toluenesulfonate (2.57 g, 10.2 mmol) was added to a solution of ethyl 4-hydroxycyclohexanecarboxylate (8.8 g, 51.10 mmol) and 3,4-dihydro-2H-pyran (8.60 g, 102 mmol) in DCM (200 mL) and the reaction was stirred at rt for 16 h. The reaction was quenched with saturated aq NaHCO3. The layers were separated and the organic layer was washed with water. The organic layer was dried (Na2SO4), filtered, and concentrated. Purification via flash chromatography on a 200 g silica column using an eluent of EtOAc in hexanes (5-10percent) afforded the title compound as a clear oil (11.1 g, 85percent).

The synthetic route of 3618-04-0 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Pfizer Inc; US2012/232083; (2012); A1;,
Ester – Wikipedia,
Ester – an overview | ScienceDirect Topics

Adding a certain compound to certain chemical reactions, such as: 135908-43-9, name is Methyl 4-aminobicyclo[2.2.2]octane-1-carboxylate hydrochloride, 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 135908-43-9, COA of Formula: C10H18ClNO2

(l-Cyano-2-ethoxy-2-oxoethylidenaminooxy)dimethylamino-mo holino-carbenium hexafluorophosphate (COMU, 1181 mg, 2.76 mmol) was added to a N,N-dimethylformamide (6 mL) solution of Hunig’s base (1.47 mL, 8.40 mmol), methyl 4-aminobicyclo[2.2.2] octane- 1- carboxylate hydrochloride (527 mg, 2.40 mmol, ArkPharm), and 2-(4-chloro-3- fluorophenoxy)acetic acid (515 mg, 2.52 mmol) that was kept stirring at 0 C. The ice bath was removed, and the reaction was left stirring at ambient temperature for 1 hour. The resulting solution was filtered through a glass microfiber frit and purified by preparative HPLC [YMC TriArt C18 Hybrid 5 mupiiota column, 50 x 100 mm, flow rate 70 mL/minute, 5-100% gradient of acetonitrile in buffer (0.1 % trifluoroacetic acid)] to give the title compound (0.78 g, 2.11 mmol, 88 % yield).JH NMR (400 MHz, DMSO-+) m/z 370 (M+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, Methyl 4-aminobicyclo[2.2.2]octane-1-carboxylate hydrochloride, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; CALICO LIFE SCIENCES LLC; ABBVIE INC.; MARTIN, Kathleen Ann; SIDRAUSKI, Carmela; FROST, Jennifer M.; TONG, Yunsong; XU, Xiangdong; SHI, Lei; XIONG, Zhaoming; (165 pag.)WO2019/90090; (2019); A1;,
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. 711-01-3, name is Methyl adamantane-1-carboxylate, A new synthetic method of this compound is introduced below., Safety of Methyl adamantane-1-carboxylate

In the 10mL single-mouth bottle,Nitrogen protection,97.1 mg (0.50 mmol) of compound 1k is added,2.5mL hexane,105.9 mg (2.25 mmol) deuterated ethanol (EtOD),129.3 mg (2.25 mmol) of sodium reagent (40 wt% dispersion in mineral oil,Particle size 5-10mum),Stir for 5 min at 0C.Rise to room temperatureThe reaction was quenched with 3.0 M aqueous hydrochloric acid.Add ether and saturated brine to extractThe organic phase is dry,Concentrate, column chromatography,79.9 mg of the target compound, 4 gYield 95%.

The synthetic route of 711-01-3 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; China Agricultural University; An Jie; Lei Peng; Han Minhui; Ma Xiaodong; Wu Yufei; A Dila¡¤adijiang; Ding Yuxuan; (15 pag.)CN107445798; (2017); A;,
Ester – Wikipedia,
Ester – an overview | ScienceDirect Topics

Application of 15448-76-7, These common heterocyclic compound, 15448-76-7, name is Dimethyl bicyclo[2.2.1]heptane-1,4-dicarboxylate, 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.

A mixture of dimethyl bicyclo[2.2.1]heptane-l ,4-dicarboxylate (1.5 g, 7.07 mmol), chromium(VI) oxide (4.24 g, 42.4 mmol) in acetic acid (15 mL) was heated at 90 C for 14 hours. The reaction mixture was diluted with ethyl acetate, washed with water, saturated NaHCC>3 and brine, dried (Na2SO/t), and concentrated. The residue was purified bychromatography eluting with 10-60% ethyl acetate in heptane to give the title compound (400 mg, 25% yield).JH NMR (400 MHz, CDC13) delta ppm 3.78 (d, J = 5.2 Hz, 6H), 2.67 (dd, J = 18.0, 2.5 Hz, 1H), 2.44 – 2.32 (m, 2H), 2.32 – 2.16 (m, 3H), 1.98 – 1.78 (m, 2H).

The synthetic route of 15448-76-7 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; CALICO LIFE SCIENCES LLC; ABBVIE INC.; MARTIN, Kathleen, Ann; SIDRAUSKI, Carmela; PLIUSHCHEV, Marina, A.; FROST, Jennifer, M.; TONG, Yunsong; BLACK, Lawrence, A.; XU, Xiangdong; SHI, Lei; ZHANG, Qingwei, I.; CHUNG, Seungwon; XIONG, Zhaoming; SWEIS, Ramzi, Farah; DART, Michael, J.; BROWN, Brian, S.; MURAUSKI, Kathleen; (673 pag.)WO2019/90069; (2019); A1;,
Ester – Wikipedia,
Ester – an overview | ScienceDirect Topics

Electric Literature of 79383-44-1, 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. 79383-44-1, name is Methyl 2-methoxy-6-methylbenzoate, This compound has unique chemical properties. The synthetic route is as follows.

N-Bromosuccinimide (250mg) and catalytic amount of 2,2′-Azobis(2- methylpropionitrile) was added to a solution of 4 (252mg) in carbon tetrachloride (3.5mL). The reaction was heated to reflux in the present of visible light for 6h. After cooling to room

The chemical industry reduces the impact on the environment during synthesis Methyl 2-methoxy-6-methylbenzoate. I believe this compound will play a more active role in future production and life.

Reference:
Patent; THE TRUSTEES OF COLUMBIA UNIVERSITY IN THE CITY OF NEW YORK; ARANCIO, Ottavio; DENG, Shixian; LANDRY, Donald, W.; FIORITO, Jole; PURGATORIO, Rosa; WO2015/153410; (2015); A1;,
Ester – Wikipedia,
Ester – an overview | ScienceDirect Topics

Synthetic Route of 148547-19-7, These common heterocyclic compound, 148547-19-7, name is Methyl 4-bromo-3-methylbenzoate, 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.

Pottasium Ferrocyanide trihydrate (3.70 g, 17.5 mmol) was added to a solution of 4-bromo-3-nnethyl-benzoic acid methyl ester (4.00 g, 17.46 mmol) in dimethylacetamide (10 ml_), followed by sodium carbonate (1 .85 g, 17.5 mmol) and palladium acetate (78 mg, 0.35 mmol). This mixture was heated at 12O0C for 15 hours, after which time it was quenched onto water (150 ml_) and extracted with tert-butylmethylether (3 x 50 ml_). The combined organic extracts were washed with water (150 ml_), dried over magnesium sulphate, filtered and evaporated under reduced pressure to give a solid (2.53 g, 83%). 1H NMR (400 MHz, CDCI3): delta 2.60 (s, 3H), 3.95 (s, 3H), 7.65 (d, 1 H), 7.95 (m, 1 H), 8.00 (d, 1 H).

Statistics shows that Methyl 4-bromo-3-methylbenzoate is playing an increasingly important role. we look forward to future research findings about 148547-19-7.

Reference:
Patent; PFIZER LIMITED; GIBSON, Karl Richard; GREEN, Martin Peter; UNDERWOOD, Toby James; WAKENHUT, Florian; WO2010/32200; (2010); A1;,
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. 454-31-9, name is Ethyl 2,2-difluoroacetate, A new synthetic method of this compound is introduced below., Recommanded Product: Ethyl 2,2-difluoroacetate

Step 2 Preparation of 4,4-difluoro-1-(3-fluoro-4-methoxyphenyl)-butane-1,3-dione Ethyl difluoroacetate (4.06 g, 32.7 mmol) was dissolved in methyl t-butyl ether (50 mL). To the stirred solution was added 25 weight % sodium methoxide (7.07 g, 32.7 mmol) followed by 3′-fluoro-4′-methoxyacetophenone (5.0 g, 29.7 mmol). After stirring for 16 hours, 1N HCl (50 mL) was added. The organic layer was collected and washed with water (2*50 mL), dried over anhydrous MgSO4, filtered, and added to hexanes to precipitate a tan solid (7.0 g, 96%): mp 70-72 C.

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; Isakson; Peter C.; Anderson; Gary D.; Gregory; Susan A.; US5700816; (1997); A;,
Ester – Wikipedia,
Ester – an overview | ScienceDirect Topics