Tag: M.W=100-200

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. 10602-03-6, name is Ethyl 4-ethynylbenzoate, This compound has unique chemical properties. The synthetic route is as follows., Product Details of 10602-03-6

General procedure: n-BuLi (4.70mL, 1.6M in hexane, 7.57mmol, 1.0equiv) was added dropwise to a solution of acetylene (7.57mmol, 1.0equiv) in 7.6mL of dry THF at -78C under a nitrogen atmosphere. After 60min at this temperature, trimethylborate (1.10g, 11.3mmol, 1.5equiv) was added dropwise at -30C. The mixture was stirred at this temperature for 60min and slowly allowed to warm to room temperature within another 60min. A saturated 4.5M aqueous solution of potassium hydrogen difluoride (KHF2) (10.1mL, 45.3mmol, 6.0equiv) was added at -20C to the vigorously stirred solution. The resulting mixture was continued to stir for 60min at -20C after which it was allowed to warm to room temperature for 60min. The solvent was removed under reduced pressure, and the resulting white solid was dried under high vacuum to remove water. The solid was washed first with acetone and then with hot acetone. The solution was concentrated to afford a white solid. The solid was dissolved in minimum amount of hot acetone, precipitated by adding methyl tert-butyl ether (MTBE), after which the solution was cooled to -20C to complete precipitation of the solid. The product was collected as an off white solid 2a-o in 40-80% yield.

According to the analysis of related databases, 10602-03-6, the application of this compound in the production field has become more and more popular.

Reference:
Article; Dubbaka, Srinivas Reddy; Nizalapur, Shashidhar; Atthunuri, Azmi Reddy; Salla, Manohar; Mathew, Thresen; Tetrahedron; vol. 70; 12; (2014); p. 2118 – 2121;,
Ester – Wikipedia,
Ester – an overview | ScienceDirect Topics

3697-68-5, name is Ethyl 1-(hydroxymethyl)cyclopropanecarboxylate, 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. Computed Properties of C7H12O3

To a solution of Preparation 232 1-hydroxymethyl-cyclopropanecarboxylic acid ethyl ester (3.00 g, 21.00 mmol) in dichloromethane (50 ml), at 0 C., was added saturated sodium hydrogen carbonate solution (50 ml), followed by TEMPO (659 mg, 4.00 mmol) and sodium bromide (400 mg, 4.00 mmol). After stirring for 5 min, sodium hypochlorite solution (10%, 14.00 mmol) was added slowly, followed by saturated sodium thiosulphate solution (50 ml). The two layers were separated and the aqueous layer was extracted with dichloromethane. The combined organic phases were dried (MgSO4) and concentrated in vacuo to give the titled compound (3.00 g). 1H-NMR (CDCl3): 1.25-1.35 (3H), 1.55-1.64 (4H), 4.21-4.30 (2H), 10.39-10.41 (1H)

The synthetic route of 3697-68-5 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Billen, Denis; Boyle, Jessica; Critcher, Douglas James; Gethin, David Morris; Hall, Kim Thomas; Kyne, Graham Michael; US2006/287365; (2006); 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. 5164-76-1, name is Dimethyl pent-2-enedioate, A new synthetic method of this compound is introduced below., SDS of cas: 5164-76-1

General procedure: The crude aryl diazonium tosylate 9 thus obtained was dissolved or suspended in MeOH (30 mL). Dimethyl glutaconate (1.45 mL, 10.0 mmol) and Pd(OAc)2 (112 mg, 0.5 mmol) were successively added while stirring. After stirring at r.t. for 15 h, the mixture was concentrated under reduced pressure and partitioned between CH2Cl2 (40 mL) and H2O (25 mL). The organic layer was washed with brine, dried (Na2SO4), and concentrated in vacuo. The residue was briefly fractionated on SiO2 using CH2Cl2 or CH2Cl2- acetone (5:1) as eluent. Fractions containing arylation product were pooled and concentrated to give compound 10 of at least 90% purity (according to 1H NMR analysis). It was used in the next step without further purification.

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:
Article; Dar’In, Dmitry; Kantin, Grigory; Bakulina, Olga; ?alubovskis, Raivis; Krasavin, Mikhail; Synthesis; vol. 51; 10; (2019); p. 2230 – 2236;,
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. 606-45-1, name is Methyl 2-methoxybenzoate, A new synthetic method of this compound is introduced below., Formula: C9H10O3

General procedure: Different substituted carboxylic acids (20 mmol) (A) were stirred with thionyl chloride (100 mmol) in dry methanol (75 ml) or 5-6 h to synthesize corresponding methyl esters (B) (Scheme1). After extraction of esters in chloroform, solvent was evaporated and esters (66 mmol) were refluxed with hydrazine hydrate(330 mmol) in ethanol (75 ml) for 4-5 h. A solid was obtained upon removal of the solvent by rotary evaporation. The resulting solid was washed with hexane to afford hydrazide ligand (C). The spectral and analytical data are given below.

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:
Article; Ain, Qurrat Ul; Ashiq, Uzma; Jamal, Rifat Ara; Mahrooof-Tahir, Mohammad; Spectrochimica Acta Part A: Molecular and Biomolecular Spectroscopy; vol. 115; (2013); p. 683 – 689;,
Ester – Wikipedia,
Ester – an overview | ScienceDirect Topics

Synthetic Route of 58656-98-7, 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 58656-98-7 as follows.

A Preparation of (26) where R10 is 2-Cyanoindole A mixture of 3.0 g (0.02 mol) of 2-cyanoindole, 4.2 g (0.02 mol) of tert-butyl-4-fluorobenzoate, and 5.5 g (0.04 mol) of potassium carbonate in 30 ml dimethyl sulfoxide was heated at 110 C. for 48 hours. The reaction was poured onto ice-water and extracted twice with ethyl acetate. The organic extracts were combined, washed with water and dried over magnesium sulfate. Evaporation yielded a dark oil which was flash chromatographed on silica gel, eluding with ethyl acetate-hexane 1:9 to give 3.6 g (0.011 mol) of 1-[4-(tertbutoxycarbonyl)phenyl]-2-cyanoindole as an oil.

According to the analysis of related databases, 58656-98-7, the application of this compound in the production field has become more and more popular.

Reference:
Patent; Syntex (U.S.A.) Inc.; US5380739; (1995); A;,
Ester – Wikipedia,
Ester – an overview | ScienceDirect Topics

Some common heterocyclic compound, 23426-63-3, name is Methyl 2-bromo-2-methylpropanoate, molecular formula is C5H9BrO2, 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. Quality Control of Methyl 2-bromo-2-methylpropanoate

A 12 L, 3 neck round bottom flask equipped with a mechanical stirrer, thermometer, condenser and nitrogen bubbler, was charged with malononitrile (251 g, 3.802 moles) and THF (2 liters). Potassium t-butoxide (1M THF, 3.802L, 3.802 moles) was then added. The mixture was stirred at 50C for 30 min. Methyl 2-bromoisobutyrate (688 g, 3.80 moles) was added and the reaction mixture was stirred overnight at 50C. The reaction was partitioned between aqueous 1 N HCI and EtOAc. The organic phase was washed with brine, dried over MgSO4, filtered, and concentrated to give the title product. 1H NMR (400 MHz, CD3CN): delta 4.35 (1 H, s) 3.73 (3 H, s), 1.43 (6 H, s).

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 23426-63-3, its application will become more common.

Reference:
Patent; MERCK SHARP & DOHME CORP.; HAN, Xiaoqing; WHITEHEAD, Alan; RAGHAVAN, Subharekha; CERNAK, Timothy, A.; DREHER, Spencer; GROEPER, Jonathan; GUO, Jian; ZHANG, Yong; WO2015/88886; (2015); A1;,
Ester – Wikipedia,
Ester – an overview | ScienceDirect Topics

Adding a certain compound to certain chemical reactions, such as: 84228-44-4, name is Methyl 4-amino-3-chlorobenzoate, 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 84228-44-4, Recommanded Product: 84228-44-4

To a solution of methyl 4-amino-3-chlorobenzoate (0.37g, 0.002 mol) and diisopropylethylamine (0.39g, 0.003 mole) in dioxane at ambient temperature was added in one portion 2-oxo-l ,2-dihydro-3-pyridinecarbonyl chloride (0.4g, 0.002 mol) [prepared as described in WO/201 1/088201 Al]. The mixture was heated at reflux for 24 h. after which it was cooled to ambient temperature and partitioned between EtOAc and water. The two phase material was filtered and the solid was washed with water, then EtOAc and air dried to obtain a 25% yield of the title compound as an off-white solid. MS: m z 305 (MIT) and m/z 307 (MH+). NMR (500 MHz, DMSO-d6): delta 3.848 (s, 3H), 6.604 (t, 1H), 7.878 (qd, 1H), 7.942 (dd, 1H), 8.015 (d, 1H), 8.504 (dd, 1H), 8.744 (d, 1H), 12.787 (br s, 1H), 12.893 (s, 1H).

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-amino-3-chlorobenzoate, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; NORTH CAROLINA CENTRAL UNIVERSITY; THE UNIVERSITY OF NORTH CAROLINA AT CHAPEL HILL; SEXTON, Jonathan Z.; BRENMAN, Jay E.; WO2014/165816; (2014); A1;,
Ester – Wikipedia,
Ester – an overview | ScienceDirect Topics

Reference of 711-01-3, These common heterocyclic compound, 711-01-3, name is Methyl adamantane-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.

Under a nitrogen atmosphere, 30.5 g (4.4 mol) of lithium metal (Li) was added to 2 L of tetrahydrofuran (THF) and stirred for 1 hour.Into this, a solution of 300 g (2.0 mol) of 2-adamantanone and 258.0 g (3.3 mol) of 2-chloropropane dissolved in 1000 mL of THF was added dropwise over 30 minutes while cooling so as to keep 20 ¡ã C. or less. .After completion of the dropwise addition, the mixture was stirred at 20 ¡ã C. for 90 minutes to obtain a THF solution of lithium 2-isopropyl-2-adamantyl alcoholate.To this THF solution, 362.0 g (2.4 mol) of methacrylic anhydride was added dropwise over 15 minutes while cooling so as to keep 20 ¡ã C. or less.After completion of the dropwise addition, the mixture was stirred at 20 ¡ã C. for 60 minutes to synthesize 2-isopropyl-2-adamantyl methacrylate.After completion of the reaction, 4 L of toluene was added, and further 2000 mL of 0.2 N aqueous NaOH solution was added, and the mixture was stirred at 20 ¡ã C. for 60 minutes.After removing the aqueous phase, washing was performed twice with 2 L of pure water.The solvent was distilled off from the organic phase to obtain 517.0 g of crude 2-isopropyl-2-adamantyl methacrylate (crude yield: 99percent, GC purity: 84.9percent).Subsequently, 0.7 g of p-methoxyphenol as a polymerization inhibitor is added to the obtained crude 2-isopropyl-2-adamantyl methacrylate,While distilling dry air from the capillary, carry out simple distillation at 0.1 kPa and 100 to 120 ¡ã C,369.0 g of distilled 2-isopropyl-2-adamantyl methacrylate (GC purity 88.2percent, referred to as ?distillate B?) was obtained.

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

Reference:
Patent; Osaka Organic Chemical Industry Ltd.; Kojima, Akio; Kono, Naoya; Uenoyama, Yoshitaka; (20 pag.)JP6478447; (2019); B2;,
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. 2216-94-6, name is Ethyl phenylpropiolate, This compound has unique chemical properties. The synthetic route is as follows., Application In Synthesis of Ethyl phenylpropiolate

General procedure: The reaction was performed in a 20-mL round-bottomed flask equipped with a Teflon-coated magnetic stirrer bar. A solution of Pd(TPP) (3.6 mg, 0.005 mumol) and DMAP (0.01 mmol, 1.2 mg) in pyridine (1 mL) was stirred at 25 C for 0.5 h under H2(1 atm, balloon). A soln of alkyne 1(0.5 mmol) in pyridine (4 mL) was added,and the mixture was stirred for the indicated time. H2O (20 mL) was added, and the aqueous phase was extracted with EtOAc (3 ¡Á 50 mL). The organic phases were combined, dried (Na2SO4), and concentrated in vacuo. The residue was purified by flash column chromatography [silica gel (20 g, 2 ¡Á 15 cm), hexane-EtOAc (40:1)] to give an alkene 2.

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 2216-94-6.

Reference:
Article; Nishibayashi, Ryo; Kurahashi, Takuya; Matsubara, Seijiro; Synlett; vol. 25; 9; (2014); p. 1287 – 1290;,
Ester – Wikipedia,
Ester – an overview | ScienceDirect Topics

927-68-4, name is 2-Bromoethyl acetate, 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. Quality Control of 2-Bromoethyl acetate

To a solution of the product of step 1(143 mg, 0.69 mmol) in DMF (1.5 mL) at 0 C, wasadded NaH (60% suspension in mineral oil, 30 mg, 0.76 mmol). The mixture was stirred for 0.5 h followed and 2-bromoethyl acetate (184 mg, 0.12 mL, 1.1 mmol) was added. The reaction was brought to room temperature and stirred overnight. The mixture was diluted with EtOAc, washed with water and brine, dried over Na2504, and concentrated underreduced pressure. The residue was purified by silica gel column chromatography (0-20% gradient MeOH in CH2C12) to afford the title compound (180 mg, 89%) as a colorless oil.?H NMR (500 MHz, CDC13) oe 1.36 (t, J=7.4 Hz, 3H), 1.89-2.00 (m, 2H), 2.03-2.15 (m, 5H), 2.75-2.82 (m, 2H), 2.89 (t, J=6.3 Hz, 2H), 3.99 (q, J=7.4 Hz, 2H), 5.25 (s, 2H)

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

Reference:
Patent; PTC THERAPEUTICS, INC.; GERASYUTO, Aleksey, I.; ARNOLD, Michael, A.; CHEN, Guangming; KARP, Gary, Mitchell; QI, Hongyan; TURPOFF, Anthony, A.; WANG, Jiashi; WOLL, Matthew, G.; BRANSTROM, Arthur, A.; NARASIMHAN, Jana; DUMBLE, Melissa, L.; HEDRICK, Jean; WEETALL, Maria, L.; (374 pag.)WO2016/109706; (2016); A1;,
Ester – Wikipedia,
Ester – an overview | ScienceDirect Topics