Month: December 2020

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 23680-40-2 as follows. SDS of cas: 23680-40-2

Methyl 3-bromopropiolate (1 13 g, 698 mmol) and freshly cracked cyclopentadiene (92 g, 1 .39 mol) were dissolved in toluene (570 ml_) and heated to 90 C, under nitrogen for 2 hr. The reaction was cooled to room temperature, and the toluene evaporated in vacuo to give a dark brown oil. This was azeotroped three times with acetonitrile to remove excess dicyclopentadiene, giving the title compound (1 19 g, 74% yield) as a brown oil. 1 H NMR (400 MHz, CDCI3) delta ppm 6.88 – 6.94 (m, 1 H), 6.85 (ddd, J = 5.2, 3.1 , 1 .0 Hz, 1 H), 4.00 (dqd, J = 2.8, 1 .7, 0.8 Hz, 1 H), 3.76 (s, 3 H), 3.69 (ddtd, J = 3.2, 2.4, 1 .5, 0.7 Hz, 1 H), 2.32 (dt, J = 6.7, 1 .7 Hz, 1 H), 2.13 (dt, J = 6.7, 1 .7 Hz, 1 H).

According to the analysis of related databases, 23680-40-2, the application of this compound in the production field has become more and more popular.

Reference:
Patent; PFIZER INC.; BURNS, Aaron Craig; COLLINS, Michael Raymond; GREASLEY, Samantha Elizabeth; HOFFMAN, Robert Louis; HUANG, Qinhua; KANIA, Robert Steven; KUNG, Pei-Pei; LINTON, Maria Angelica; NARASIMHAN, Lakshmi Sourirajan; RICHARDSON, Paul Francis; RICHTER, Daniel Tyler; SMITH, Graham; WO2015/166373; (2015); A1;,
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Synthetic Route of 178312-47-5,Some common heterocyclic compound, 178312-47-5, name is Ethyl 4,4-difluorocyclohexanecarboxylate, molecular formula is C9H14F2O2, 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 solution ofbutyllithium(2.000 mL, 2.80 mmol) was added to a cold (-78 C.) solution ofdiisopropylamine(0.396 mL, 2.80 mmol) inTHF(5 mL) under N2and the mixture was stirred at -78 C. for 1 h. A solution ofethyl 4,4-difluorocyclohexanecarboxylate(384 mg, 2 mmol) in THF (2 mL) was added at -78 C. and the mixture was stirred for 1 h and then gradually warmed to -20 C. over 2 h and then re-cooled to -78 C. Neat((chloromethoxy)methyl)benzene(0.226 mL, 2.200 mmol) was added and the mixture was allowed to warm to rt over 2 h. The reaction was quenched with satd. NH4Cl and extracted with EtOAc and washed with water, brine, dried (Na2SO4). Evaporation of the solvent afforded a lightyellowoil which was purified by silica gel FCC (1:1 DCM-hexanes) to afford1-((benzyloxy)methyl)-4,4-difluorocyclohexanecarboxylateas acolorlessoil.

The synthetic route of 178312-47-5 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Hewawasam, Piyasena; Lopez, Omar D.; Tu, Yong; Wang, Alan Xiangdong; Xu, Ningning; Kadow, John F.; Meanwell, Nicholas A.; Gupta, Samayamuthula Venkata Satya Arun Kumar; Kumar, Indasi J. Gopi; Ponugupati, Suresh Kumar; Belema, Makonen; US2015/23913; (2015); A1;,
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3196-23-4, name is Methyl 1-bromocyclohexanecarboxylate, belongs to esters-buliding-blocks compound, is considered to be a conventional heterocyclic compound, which is widely used in drug synthesis. The chemical synthesis route is as follows. COA of Formula: C8H13BrO2

To a suspension of chromium (II) chloride (1. 00 g, 8. 10 MMOL) and lithium iodide (0. 087 G, 0. 648 MMOL) in tetrahydrofuran (20 mL) was added 4- [2- (5-METHYL-2- phenyl-1, 3-oxazol-4-yl) ethoxy] BENZALDEHYDE (Preparation 1) (1. 00 g, 3. 24 MMOL) and methyl 1-bromocyclohexanoate (1. 07 g, 4. 85 MMOL). The resulting mixture was heated at 50 C until TLC analysis indicated the reaction was complete. The mixture was cooled to ambient temperature and satuarted aqueous sodium chloride (15 mL) was added. The resulting mixture was stirred for 15 minutes, then partitioned between water and ethyl acetate. The organic phase was washed with water and dried (anhydrous magnesium sulfate), filtered and evaporated. The residue was purified by flash column chromatography (hexanes to 50% ethyl acetate/hexanes) to yield the title compound as a colorless oil (0. 797 G, 55%). LRMS (M/Z) : 450 (M+H).

The synthetic route of 3196-23-4 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; PFIZER INC.; WO2004/92145; (2004); A1;,
Ester – Wikipedia,
Ester – an overview | ScienceDirect Topics

Related Products of 91367-05-4, 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 91367-05-4 as follows.

To a solution of methyl 4-chloro-3-methylbenzoate (2.22 g, 12 mmol) in CCl4 (16 mL) was added NBS (2.35 g, 13.2 mmol) and AIBN (0.031 g, 0.19 mmol) and the reaction was refluxed for 3 h. After cooled down, the reaction was filtered and the filtrate was washed with H2O, dried over N yi 3H), 4.628 (s, 2H,), 7.494 (d, IH, /=8.4 Hz), 7.942 (d, IH, /=8.4 Hz), 8.143 (s, IH).

According to the analysis of related databases, 91367-05-4, the application of this compound in the production field has become more and more popular.

Reference:
Patent; SMITHKLINE BEECHAM CORPORATION; WO2007/65093; (2007); 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. 924-99-2, name is Ethyl 3-(dimethylamino)acrylate, This compound has unique chemical properties. The synthetic route is as follows., Recommanded Product: Ethyl 3-(dimethylamino)acrylate

220g of toluene, 95g of triethylamine, 200g acid chloride sequentially into the acylation reactor, open stirring, cooling to 13 ;Preparation of the first 98g N, N-dimethylamino ethyl acrylate added to the dropping device, keeping the reaction kettle temperature 12 open stirring dropping,25 minutes to complete all the dropwise addition is completed, slowly heated to 75 C and incubated for 6 hours; step is completed, cooled to20 C, into 60g L-aminopropanol, slowly heated to 45 C, incubated for 3 hours, was added 200g saturated brine,Slowly add dropwise adjust PH5.5, stirring for 20 minutes, retest PH value after stopping stirring Stirred stratification, toluene layer decompression recovery of tolueneNo toluene solution into the reactor, pumped DMF200g stirring dissolved into the ring reactor high tank to be used; to the reaction within the reactorInto DMF1500g, start stirring, cast KF130g, temperature and pressure before recovery fraction to the reactor temperature 160 . Add amineThe reaction solution was heated to maintain refluxing heat 4 hours; end of the insulation, cooling to below 100 , DMF was recovered under reduced pressureWill be dry. After the end of the recovery of high pure water 1200g, stirred for 40 minutes, filtered, washed with water, finally rinsed with methanol, dried, too176g product, 96.8% molar yield.

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 924-99-2.

Reference:
Patent; Yancheng Xin’an Zhou Pharmaceutical Co., Ltd.; Chen Chengle; Zhang Wenbiao; (6 pag.)CN106565745; (2017); A;,
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. 35613-44-6, name is Methyl 2-(2-aminophenyl)acetate, A new synthetic method of this compound is introduced below., COA of Formula: C9H11NO2

Methyl 2- (2-aminophenyl) acetate (0.71 g, 4.3 mmol) andSodium carbonate (0.16g, 1.6mmol)Dissolved in tetrahydrofuran (10mL),Reduce the temperature to -78 and stir for 1h.2-bromopropionyl chloride (0.77g, 4.5mmol) andTetrahydrofuran (5mL) was mixed slowly and completely within 0.5 hours.After the addition is complete, move to room temperature and stir for 5h.Methyl 2- (2- (2-bromopropionamide) phenyl) acetate (white solid, 1.16 g) was obtained in a yield of 90%.

The synthetic route of 35613-44-6 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Zhangzhou Sanitation Profession College; Zheng Lulu; Luo Jinhong; Yang Lina; Chen Tongjun; (7 pag.)CN110272351; (2019); A;,
Ester – Wikipedia,
Ester – an overview | ScienceDirect Topics

Adding a certain compound to certain chemical reactions, such as: 653-92-9, name is Methyl 2-bromo-4-fluorobenzoate, 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 653-92-9, Product Details of 653-92-9

a) 2-Bromo-4-dimethylamino-benzoic acid methyl ester (7a) To a stirred solution of 5,24 g (22.5 mmol) 2-Bromo-4-fluoro-benzoic acid methyl ester (Rarechemicals) and 60.0 ml dimethylsulphoxid are added 2.23 g (27.0 mmol) dimethylamine hydrochloride and 6.54 g (47.3 mmol) potassium carbonate. The reaction mixture is stirred for 11h at 70C in an autoclave and is concentrated with high vacuum rotation evaporator at 65C. The residue is diluted with dichloromethane, washed twice with water. The combined water phases are extracted with dichloromethane. The combined dichloromethane phases are washed with diluted sodium hydrogen carbonate solution, dried with sodium sulphate and concentrated. The oily crude is purified by column chromatography and the desired product 7a is obtained in 70 % yield (4,08 g, 15.8 mmol). MS-ESI: 258/560 (M+ +1, 88/83).

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; Bayer Schering Pharma Aktiengesellschaft; EP1897885; (2008); A1;,
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. 99548-54-6, name is Methyl 3-bromo-2-methylbenzoate belongs to esters-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below. Product Details of 99548-54-6

A mixture of 3-Bromo-2-methyl benzoic acid methyl ester (2.4 g, 10.29 mmol), NBS (1.83 g, 10.29 [MMOL)] and AIBN (4 mg) in [CHLOROBENZENE] (40 mi) was heated to [80C] under nitrogen for 18 hours. The mixture was cooled in an ice-bath, filtered and the solvent removed by evaporation under reduced pressure. The orange residue was purified by flash chromatography on silica gel eluting with a solvent gradient of heptane: ethyl acetate (40: 1) to give the title compound (2.74 g, 86 %) as a colourless oil. [1H-NMR] (400 MHz, [CDCI3)] : [ES] = 3.88 (s, 3H), 5.06 (s, 2H), 7.22 (dd, 1H), 7.68 (d, [1H),] 7. 89 (d, [1 H).] Microanalysis : Found: C, 35.21 ; H, 2.67 ; N, 0.00. [C9H8BR202] requires C, 35.10 ; H, 2.62 ; N, 0.00%.

The synthetic route of 99548-54-6 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; PFIZER LIMITED; PFIZER INC.; WO2004/14357; (2004); A2;,
Ester – Wikipedia,
Ester – an overview | ScienceDirect Topics

Application of 35065-86-2, 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. 35065-86-2, name is 3-Bromophenyl acetate belongs to esters-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

General procedure: A stirred solution of the appropriate bromophenyl alkanoic acid(1 eq) in MeOH (25 mL)was treated with H2SO4 (0.1 eq of a conc. aq.solution) and heated at reflux for 18 h. The resultant solution wascooled to room temperature and concentrated under reducedpressure. The resultant oil was diluted with NaHCO3 (50 mL of a sat.aq. solution) and subsequently extracted with diethyl ether(3 25 mL). The combined organics were washed with brine(1 100 mL), dried (MgSO4), filtered and concentrated underreduced pressure to give the desired methyl ester:

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

Reference:
Article; Jorgensen, William T.; Gulliver, Damien W.; Katte, Timothy A.; Werry, Eryn L.; Reekie, Tristan A.; Connor, Mark; Kassiou, Michael; European Journal of Medicinal Chemistry; vol. 143; (2018); p. 1644 – 1656;,
Ester – Wikipedia,
Ester – an overview | ScienceDirect Topics

Reference of 927-68-4, These common heterocyclic compound, 927-68-4, name is 2-Bromoethyl acetate, 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.

Dissolve ethyl imidazole-2-carboxylate (200 mg, 1.43 mmol) in 5 ml of N,N-dimethylformamide, add cesium carbonate (931 mg, 2.85 mmol) and activate for 0.5 h, then add2-bromoethyl acetate(385mg, 2.14mmol), warmed to 80C for 2h, complete reaction by TLC, stop reaction, cooled to room temperature, diluted with water, extracted with ethyl acetate (3¡Á20ml), combined organic layers, washed with saturated brine, anhydrous Dry over sodium sulfate, filter, and concentrate to obtain crude product. Purified by column chromatography (PE:EA=3:1) to give a pale yellow liquid, namely compound 1-(2-acetoxyethyl)-1H-imidazole-2-carboxylic acid ethyl ester 26b (300mg, yield 92.8 %).

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

Reference:
Patent; Sichuan University; Li Guobo; Wang Zhenling; (40 pag.)CN111187218; (2020); A;,
Ester – Wikipedia,
Ester – an overview | ScienceDirect Topics