Tag: M.W=200-300

Related Products of 2672-58-4, 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. 2672-58-4, name is Trimethyl benzene-1,3,5-tricarboxylate belongs to esters-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

Preparation 1 1,3,5-Tris(hydroxymethyl)benzene A solution of trimethyl 1,3,5-benzenetricarboxylate (8.83 g, 0.035 M; Aldrich) in THF (125 mL) is added dropwise over a period of 45 minutes to a stirred mixture of lithium aluminum hydride (3.98 g, 0.105 M) and dry THF (150 mL) under a nitrogen atmosphere. The initial phase of the addition results in vigorous reaction and consequently the addition is very slow at first. As the ester solution is added, an orange mass forms when the drops came in contact with the LiAlH4 mixture. A yellowish-green mixture results and is stirred at room temperature. The excess LiAlH4 is quenched carefully by the addition of ethyl acetate and the resulting mixture is acidified with aqueous 2N HCl solution until the pH is <3 and aluminum salts have dissolved. The layers are separated and the aqueous layer is extracted 3 times with additional ethyl acetate and then with methylene chloride. The organic extract layers are dried (sodium sulfate), filtered, and concentrated under reduced pressure to give a white solid (2.98 g, 51%). Recrystallization from acetonitrile-methylene chloride gives the title compound as white crystals (1.13 g) which appear to be hygroscopic when collected by suction filtration. The crystals are dried several days over P2 O5 in a vacuum desiccator after which they have amp of 76.5-78 C. 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, Trimethyl benzene-1,3,5-tricarboxylate, other downstream synthetic routes, hurry up and to see. Reference:
Patent; The Upjohn Company; US5500417; (1996); A;,
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These common heterocyclic compound, 141772-31-8, name is Methyl 5-amino-2-chloro-4-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. COA of Formula: C8H7ClFNO2

2. Preparation of Compound No. 18 A solution of 2-fluoro-4-chloro-5-methoxycarbonylaniline (1.0 g, 5 mmol) in THF (10 mL) was added dropwist to a solution of diphosgene (2.0 g, 10 mmol) in toluene (20 mL) with stirring at room temperature. The reaction mixture was stirred at room temperature for one hour and then heated to reflux for 4 hours. The mixture was then cooled to room temperature and the solvents were evaporated under reduced pressure to give 1.1 g of 2-fluoro-4-chloro-5-methoxycarbonylphenyl isocyanate as a solid.

The synthetic route of Methyl 5-amino-2-chloro-4-fluorobenzoate has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Dow AgroSciences LLC; US6444615; (2002); B1;,
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Application of 13078-21-2, 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. 13078-21-2, name is Ethyl 2-(2-methoxyphenoxy)acetate belongs to esters-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

rytftro-l-(4-hydroxy-3-methoxyphenyl)-2-(2-methoxyphenoxy)-l,3- propanediol (2h): (0183) (0184) 2h (0185) Scheme 9. Synthesis of ?’r_yi zro-l-(4-hydroxy-3-methoxyphenyl)-2-(2- methoxyphenoxy)– 1 ,3-propanediol (2h). (0186) This compound was prepared according to the same literature procedure as for compound 2g. Spectral data were consistent with those reported in the literature. JH NMR (400 MHz, CDC13) delta 7.16 (dd, J = 8.2, 1.6 Hz, 1H), 7.04-6.86 (m, 5H), 6.86 (d, J = 8.2 Hz, 1H), 5.71 (b s 1H), 4.96 (d, J = 7.9 Hz, 1H), 4.06-3.97 (m, 1H), 3.90 (s, 3H), 3.87 (s, 3H), 3.73-3.58 (m, 2H), 3.48 (ddd, J = 12.0, 7.8 and 3.6 Hz, 1H), 2.78-2.73 (m, 1H). HRMS (ESI) calculated for CnHzoOeNa [M + Na]+ 343.1158, found 343.1154.

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, Ethyl 2-(2-methoxyphenoxy)acetate, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; WISCONSIN ALUMNI RESEARCH FOUNDATION; STAHL, Shannon, S.; COON, Joshua; RAHIMI, Alireza; ULBRICH, Arne; WO2015/138563; (2015); A1;,
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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. 1150164-80-9, name is Ethyl 2,2-difluoro-2-(2-methoxyphenyl)acetate, This compound has unique chemical properties. The synthetic route is as follows., Safety of Ethyl 2,2-difluoro-2-(2-methoxyphenyl)acetate

General procedure: To a solution of an appropriate ethyl alpha,alpha-difluoroaryl acetate (1.0 eq.) in MeOH (0.33 M) was added 1 M aq. K2CO3 (3.0 eq.). The reaction mixture was stirred at room temperature for 12 h before diluting with Et2O. The reaction mixture was extracted with aq. NaHCO3 (sat., 3x). The combined aqueous layers were acidified to pH 1 and extracted with Et2O (3x), then the combined organic phases were washed with brine, dried over MgSO4 and concentrated in vacuo. Products were purified by washing with n-pentane.

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 1150164-80-9.

Reference:
Article; Verhoog, Stefan; Pfeifer, Lukas; Khotavivattana, Tanatorn; Calderwood, Samuel; Collier, Thomas Lee; Wheelhouse, Katherine; Tredwell, Matthew; Gouverneur, Veronique; Synlett; vol. 27; 1; (2016); p. 25 – 28;,
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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. 41727-48-4, name is Methyl 4-amino-3,5-dichlorobenzoate, A new synthetic method of this compound is introduced below., Safety of Methyl 4-amino-3,5-dichlorobenzoate

Example 45 Preparation of methyl 3,5-dichloro-4-cyanobenzoate (C77) Copper(I) cyanide (7.41 g, 82.7 mmol) was added to acetonitrile and heated to 80 C. for 30 minutes. tert-Butyl nitrite (10.5 g, 102 mmol) was added followed by methyl 4-amino-3,5-dichloro-benzoate (14.0 g, 63.6 mmol) in acetonitrile (200 mL) and the reaction mixture was stirred at 80 C. for 30 minutes. The reaction mixture was poured into an ammonia solution and extracted with petroleum ether to provide the title compound as an off-white solid (7.00 g, 43%): mp 98-101 C.; 1H NMR (400 MHz, CDCl3) delta 8.12 (s, 2H), 3.98 (s, 3H); ESIMS m/z 229 ([M+H]+).

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; Dow AgroSciences LLC; LePlae, JR., Paul R.; Barton, Thomas; Gao, Xin; Hunter, Jim; Lo, William C.; Boruwa, Joshodeep; Tangirala, Raghuram; Watson, Gerald B.; Herbert, John; (147 pag.)US2017/210723; (2017); 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. 2905-69-3, name is Methyl 2,5-dichlorobenzoate, A new synthetic method of this compound is introduced below., Recommanded Product: 2905-69-3

EXAMPLE 2 Dehalogenation of Methyl 2,5-Dichlorobenzoate A 50-mL round-bottom flask was equipped with a magnetic stir bar, reflux condenser, thermometer, nitrogen inlet, and heating mantle attached to a temperature controller. The flask was charged with methyl 2,5-dichlorobenzoate (5.0 g, 24 mmol) and copper powder (3.04 g, 48 mmol). Propionic acid (10 mL) and xylenes (15 mL) were added, and the resulting mixture was heated to 130-135 C. The reaction was monitored by GC analysis and was judged to be complete when the starting material was no longer detectable (3 hours). The reaction mixture was cooled to room temperature and filtered; the solids were washed with xylenes. The filtrates were blue-green. The filtrates were combined and washed with 1M hydrochloric acid solution until the blue-green color disappeared. The resulting yellow organic layer was washed with water and dried over sodium sulfate. The solvent was removed by evaporation under reduced pressure. The residue was dried under vacuum, yielding 3.93 g of methyl 3-chlorobenzoate as a pale yellow oil.

The synthetic route of 2905-69-3 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Rohm and Haas Company; US5886210; (1999); A;,
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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. 57486-69-8, name is Methyl 2-(2-bromophenyl)acetate, This compound has unique chemical properties. The synthetic route is as follows., Formula: C9H9BrO2

Degas a suspension of methyl 2-(2-bromophenyl)acetate (156.6 g, 684 Tnmoi), bis(inacoiato)diboron (194.9 g, 752 mmoi), and potassium acetate (135,6 g, 1.4 mol) in N-methylpyrroiidone (940 mL) with three vacuuni?nitrogen cycles, Add (1,1 bis(diphenyiphosphino)ferrocene)palladiurn(H) chloride (11,4 g, 13,7 nunol) and heat at 80C. After 15 hours add (1 , I -bis(diphenyiphosphino)ferrocene)palladiuni(II) chloride(11,4 g, 13.7 mmoi) and stir at 90 C for 24 hours, Cool to ambient tern perare and pour over a mixture of ice and water (3 L), and methyl tertiary butyl ether (1 L) was added, Stir mixture, filter through a pad of Celite and separate layers, Extract from aqueous with methyl tertiary hutyl ether (2×500 niL), Wash combined organics with water (2×500 mL), brine (500 mL), dry over sodium sulfate and concentrate. Purify the residue byflash chromatography, elating with hexane: ethyl acetate (9:1) to give the title compound as a white solid (160,6 g, 581.6 mrnol, 85%). MS (rn/z): 277(M+i),

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 57486-69-8.

Reference:
Patent; ELI LILLY AND COMPANY; BENHADJI, Karim A.; MASSARD, Christophe; SORIA, Jean-Charles; (43 pag.)WO2016/168014; (2016); A1;,
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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 89901-03-1 as follows. SDS of cas: 89901-03-1

Example 97; (4′ -Bromo-biphenyl-4-yl) -methanol; A solution of 4′ -Bromo-biphenyl-4-carboxylic acid methyl ester, 7.8g (27.9′ mmol) in 15OmL of tetrahydrofuran was cooled to 0 0C via ice-water bath. Lithium aluminum hydride, l.lg (27.9 mmol) was added to the solution in one portion. The reaction mixture stirred at 0 0C for Ih. The mixture was slowly quenched with 1OmL of isopropyl alcohol, then with 1OmL of water. The aqueous mixture was extracted with 3x50mL portions of ethyl acetate. The organic layers were combined, washed with sat. aq. NaCl, and dried (MgSO4) . The solution was concentrated to afford the desired product in 7.01g (100%) as a white solid. The material was taken to the next step without further purification.

According to the analysis of related databases, 89901-03-1, the application of this compound in the production field has become more and more popular.

Reference:
Patent; THE INSTITUTES FOR PHARMACEUTICAL DISCOVERY, LLC; WO2006/55725; (2006); A2;,
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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 914943-91-2 as follows. SDS of cas: 914943-91-2

-Butyl 3-ethynyibenzoate (117) (1.603 g, 7.93 mmol), 4-iodo-2-(methylthio)-5- (trifiuoromethyl)pyrimidine (114) (1.647 g, 5.15 mmol), PdCI2(PPh3)2 (0.316 g, 0.45 mmoi), PPh3 (0.355 g, 1.35 mmol), Cu(i)i (0.232 g, 1.22 mmol) and trethyiamine (4.00 mL, 28.7 mmoi) were combined in D F (20 mL) and the resulting mixture heated at 120 C under microwave irradiation for 25 minutes. The mixture was then concentrated under reduced pressure and purified twice using silica gel column chromatography (10-20% EtOAc/petroleum benzine 40-60 C then 50-100% DCM/petroleum benzine 40-60 C) to give the title compound (118) (0.624 g, 31 %) as a yellow solid; 1H NMR (400 MHz, CDCI3) delta 8.73 (d, J = 0,8 Hz, H), 8.25 (m, H), 8.08 (m, 1 H), 7.78 (m, 1 H), 7.48 (m, 1 H), 2.63 (s, 3H), 1.61 (s, 9H).

According to the analysis of related databases, 914943-91-2, the application of this compound in the production field has become more and more popular.

Reference:
Patent; CANCER THERAPEUTICS CRC PTY LTD; DEVLIN, Mark Graeme; STREET, Ian Philip; TONG, Warwick Bonner; WO2014/27199; (2014); A1;,
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Related Products of 6942-39-8, A common heterocyclic compound, 6942-39-8, name is Methyl 2-bromo-5-fluorobenzoate, molecular formula is C8H6BrFO2, 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.

To a solution of methyl 2-bromo-5-fluorobenzoate (18.26 moles) in DMF (total vol. 9.2 L) was charged copper(I) cyanide (1.603 kg) in DMF (5 L) slurry and followed with a DMF flush (4 L). After being degassed, the reaction mixture was heated at 100 C. for 10-16 hours. The reaction mixture was monitored by HPLC (conversion was >98%). After being cooled to 50 C.-60 C., ethyl acetate (20 L) was added, and then 10% NH4OH-20% NH4Cl (22 L). The mixture was then transferred to a 100 L nalgene extractor. The 72 L round bottom flask was washed with 15 L of EtOAc and 15 L of water and transferred to the 100 L extractor. After phase cut, the aqueous layer was back-extracted with EtOAc (17 L) one time. The combined organic layers were washed with 10% NH4OH/20% NH4Cl:water (1:1, 3*10 L), 16% brine (8 L), concentrated, and solvent switched to MeOH (total vol. 22 L, KF=152.6 mug/mL). The resulting solution was used for next step. HPLC conditions: column: Zorbax, Rx C8 250*4.6 mm; temperature: 30 C.; detection at 210 nm; mobile phase: 0.1% aq H3PO4 (A)/MeCN (B); gradient: 90:10 (A)/(B) to 10:90 over 15 min, 10:90 hold for 5 min, 10:90 to 90:10 (A)/(B) over 10 seconds; flow rate: 1 mL/min; retention time for the desired monoester: 11.7 min. Evaporation of a sample to dryness gave a light yellow solid: 1H NMR (CDCl3) delta: 7.86-7.80 (m, 2H), 7.37 (td, J=8.5, 2.6 H, 1H), 4.02 (s, 3H); 13C NMR (100 MHz, CDCl3) delta: 164.3 (d, J=260 Hz), 163.3, 137.1 (d, J=10.0 Hz), 135.2 (d, J=10.0 HZ), 120.2 (d, J=30.0 Hz), 118.8 (d, J=20.0 Hz), 116.6, 109.0, 53.1.

The synthetic route of 6942-39-8 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Lee, Jaemoon; Zhong, Yong-Li; US2004/220273; (2004); A1;,
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