Month: July 2021

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. 29823-21-0, name is Ethyl 8-Bromooctanoate, This compound has unique chemical properties. The synthetic route is as follows., Recommanded Product: 29823-21-0

EXAMPLE 76 Ethyl 8-(4-phenylimidazol-1-yl)octanoate 4-Phenylimidazole was treated with ethyl 8-bromooctanoate and potassium carbonate in butanone to give after work-up the title compound, m.p. 56-57 C., Found: C, 72.8; H, 8.4; N, 9.0%; C19 H26 N2 O2 Requires: C, 72.6; H, 8.3;N, 8.9%

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 29823-21-0.

Reference:
Patent; SmithKline Beecham Corporation; The Johns Hopkins University; US5648373; (1997); A;,
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Reference of 4518-10-9, A common heterocyclic compound, 4518-10-9, name is Methyl 3-aminobenzoate, molecular formula is C8H9NO2, 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 B-14a (1 eq.) in toluene is added Ac20 (1.05 eq.) dropwise at reflux and the mixture is stirred at reflux for several minutes. The product B-15a can be crystallized out of the mixture by cooling down and further dilution.

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; BOEHRINGER INGELHEIM INTERNATIONAL GMBH; GOLLNER, Andreas; BROEKER, Joachim; KERRES, Nina; KOFINK, Christiane; RAMHARTER, Juergen; WEINSTABL, Harald; GILLE, Annika; GOEPPER, Stefan; HENRY, Manuel; HUCHLER, Guenther; (365 pag.)WO2017/60431; (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. 344-14-9, name is Dimethyl 2-fluoromalonate, A new synthetic method of this compound is introduced below., Recommanded Product: Dimethyl 2-fluoromalonate

Sodium hydride (60% dispersion in mineral oil; 2.93 g, 73.3 mmol) was added to a solution of dimethyl 2-fluoromalonate (10.0 g, 66.6 mmol) in THF (218 mL) with vigorous stirring. After 30 minutes iodomethane (4.56 mL, 73.3 mmol) was added. The reaction was stirred for a further 3 hours. The reaction was quenched with water and then extracted with EtOAc (4*100 mL). The combined organic layers were dried over Na2SO4, filtered, and concentrated under reduced pressure to afford dimethyl 2-fluoro-2-methyl-propanedioate (8.4 g, 77%) as an orange oil. 1H NMR (300 MHz, DMSO-d6, 27 C.) 1.72 (3H, d), 3.77 (6H, s).

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; AstraZeneca AB; BARLAAM, Bernard Christophe; O’DONOVAN, Daniel Hillebrand; HUGHES, Samantha Jayne; MOSS, Thomas Andrew; NISSINK, Johannes Wilhelmus Maria; SCOTT, James Stewart; YANG, Bin; (148 pag.)US2018/111931; (2018); 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. 383-62-0, name is Ethyl 2-chloro-2,2-difluoroacetate, A new synthetic method of this compound is introduced below., name: Ethyl 2-chloro-2,2-difluoroacetate

EXAMPLE 18 Synthesis of 1-chloro-4-cyclohexyl-1,1-difluoro-2,4-butanedione STR27 74.8 g of sodium methoxide was added to 1l of ethyl ether, and a solution of 200 g of ethyl chlorodifluoroacetate in 300 ml of ethyl ether was dropwise added thereto under stirring at 0 C. Then, a solution of 106 g of cyclopropyl methyl ketone in 300 ml of ethyl ether was gradually dropwise added to the reaction solution, and after completion of the dropwise addition, the mixture was stirred at room temperature for 8 hours. The solvent was distilled off under reduced pressure, 300 ml of 6N hydrochloric acid was added to the residue, and extraction with ethyl acetate was carried out. The extract layer was washed with water, and the solvent was distilled off under reduced pressure to obtain 235.9 g of the desired product as a pale yellow liquid. Refractive index nD20.6 1.4788

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; Nissan Chemical Industries, Ltd.; US5716904; (1998); A;,
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Electric Literature of 37746-78-4, A common heterocyclic compound, 37746-78-4, name is (E)-Ethyl 4-bromobut-2-enoate, molecular formula is C6H9BrO2, 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.

An ethanol solution of 9A- THC (1) (100 mg, 0.318 mmol) was transferred to a round bottom flask (Figure 5). The original vial was washed with methanol and the washes added to the flask. Next the solvent was removed on the rotary evaporator, to give yellow oil. The isolated 9A-THC yellow oil was dissolved in 10 mL acetone (dried over K2CO3) followed by the addition of 0.45 g potassium carbonate (3.2 mmol). Ethyl 4- bromocrotomate (118 uL, 165 mg x 75% = 124, 0.64 mmol, 2 eq.) was then added to the mixture. This RT reaction was stirred overnight, under argon. In the morning, the reaction was analyzed by TLC (silica gel, 10:1 hexanes-ethyl acetate, visualization with UV). The TLC indicated a complete reaction, the starting material having been consumed and a new spot having formed at a higher i?/from the starting material. Next, the solid was filtered off through a bed of CELITE. The solid was then washed with acetone (2 x 10 mL). The filtrate was concentrated to give very light yellow oil. This residue was then purified by preparative TLC on a silica gel using hexanes-ethyl acetate 10:1 as eluent. The top band (R/= 0.57) was collected to give 135 mg (99%) of the desired product 21 as a clear oil.

The synthetic route of 37746-78-4 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; OAKVILLE HONG KONG COMPANY LIMITED; WO2006/29089; (2006); A2;,
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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. 37746-78-4, name is (E)-Ethyl 4-bromobut-2-enoate belongs to esters-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below. COA of Formula: C6H9BrO2

General procedure: To a vigorously stirring solution of alpha-imino ester 1 (0.5 mmol,1 equiv) and E-ethyl-4-bromocrotonate or methyl-4-bromocrotonate (2, 1.5 mmol, 3 equiv) in EtOH (2 mL) was added indium powder (1 mmol, 2 equiv). The mixture was allowed to stir vigorously for 6 h at 30 C. After this period, the reaction mixturewas quenched with 2 mL of water and transferred to a separating funnel and extracted using ethyl acetate (315 mL). The combined organic layers were dried over anhydrous Na2SO4. Then the solvent was evaporated under vacuum. Purification of the resulting crude reaction mixture by column chromatography on silica gel (EtOAc/Hexane as eluent) gave the product 3 (see Tables 1 and 2 and Scheme 2 for individual entries).

The synthetic route of 37746-78-4 has been constantly updated, and we look forward to future research findings.

Reference:
Article; Aslam, Nayyar Ahmad; Babu, Srinivasarao Arulananda; Sudha, Arya Jayadev; Yasuda, Makoto; Baba, Akio; Tetrahedron; vol. 69; 32; (2013); p. 6598 – 6611;,
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Application of 1195768-18-3,Some common heterocyclic compound, 1195768-18-3, name is Methyl 3-amino-2-fluorobenzoate, molecular formula is C8H8FNO2, 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 A: methyl 3-{[(2,6-difluorophenyl)sulfonyl]amino}-2-fluorobenzoate Methyl 3-amino-2-fluorobenzoate (50 g, 1 eq) was charged to reactor followed by dichloromethane (250 mL, 5 vol). The contents were stirred and cooled to ~15C and pyridine (26.2 mL, 1.1 eq) was added. After addition of the pyridine, the reactor contents were adjusted to ~15C and the addition of 2,6-diflurorobenzenesulfonyl chloride (39.7 mL, 1.0 eq) was started via addition funnel. The temperature during addition was kept <25C. After complete addition, the reactor contents were warmed to 20-25C and held overnight. Ethyl acetate (150 mL) was added and dichloromethane was removed by distillation. Once distillation was complete, the reaction mixture was then diluted once more with ethyl acetate (5 vol) and concentrated. The reaction mixture was diluted with ethyl acetate (10 vol) and water (4 vol) and the contents heated to 50-55C with stirring until all solids dissolve. The layers were settled and separated. The organic layer was diluted with water (4 vol) and the contents heated to 50-55 for 20-30 min. The layers were settled and then separated and the ethyl acetate layer was evaporated under reduced pressure to ~3 volumes. Ethyl Acetate (5 vol.) was added and again evaporated under reduced pressure to ~3 volumes. Cyclohexane (9 vol) was then added to the reactor and the contents were heated to reflux for 30 min then cooled to 0 C. The solids were filtered and rinsed with cyclohexane (2 x 100 mL). The solids were air dried overnight to obtain methyl 3-{[(2,6-difluorophenyl)sulfonyl]amino}-2-fluorobenzoate (94.1 g, 91%). These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route Methyl 3-amino-2-fluorobenzoate, its application will become more common. Reference:
Patent; GLAXOSMITHKLINE INTELLECTUAL PROPERTY (NO.2) LIMITED; GRESHOCK, Joel David; HOOS, Axel; WO2015/87279; (2015); A1;,
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These common heterocyclic compound, 924-99-2, name is Ethyl 3-(dimethylamino)acrylate, 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. HPLC of Formula: C7H13NO2

General procedure: Ethyl 4-(4-chlorophenyl)-2-thioxo-1,2,3,4-tertahydropyrimidine-5-carboxylate 6a (Table 2, entry 1). To a mixture of thiourea 12a (23.0 mg, 0.302 mmol), 4-chlorobenzaldehyde 13a (63.0 mg, 0.448 mmol), and ethyl 3-dimethylaminoacrylate 9 (64.0 mg, 0.447 mmol) in anhydrous DMF (0.3 mL) was added anhydrous aluminum chloride (8.0 mg, 0.0600 mmol) at room temperature, and the reaction mixture was stirred at 110 C for 3 h. To the mixture was added EtOAc (10 mL) and 1 M HCl aqueous solution (5 mL), and the organic layer was separated. The aqueous layer was extracted with EtOAc (10 mL), and the combined organic layers were washed with water (5 mL) and brine (5 mL), dried over anhydrous MgSO4, and concentrated under reduced pressure. The residue was purified by silica gel column chromatography [n-hexane-EtOAc (4:1 to 2:1)] to give 6a (78.9 mg, 0.266 mmol, 88%) as pale yellow crystals.

The synthetic route of Ethyl 3-(dimethylamino)acrylate has been constantly updated, and we look forward to future research findings.

Reference:
Article; Arai, Rie; Cho, Hidetsura; Gokurakuji, Yuki; Kikuchi, Hidetomo; Kubo, Takanori; Nakamura, Yuri; Nishimura, Yoshio; Sunaga, Katsuyoshi; Yuan, Bo; Tetrahedron Letters; (2020);,
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Application of 3153-37-5, 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. 3153-37-5, name is Methyl 4-chlorobutyrate, This compound has unique chemical properties. The synthetic route is as follows.

Step A: 1-(S)-(1-(R)-(3,5-Bis(trifluoromethyl)phenyl)ethoxy)-2-(R)-(4-fluorophenyl)-3-(R)-(((3-methoxycarbonylpropyl)methylamino)methyl)cyclopentane To a solution of 65 mg of 1-(S)-(1-(R)-(3,5-bis(trifluoromethyl)phenyl)ethoxy)-2-(R)-(4-fluorophenyl)-3-(R)-((methylamino)methyl)cyclopentane from Example 18, Step B in 1 mL of acetonitrile was added 0.019 mL of methyl 4-chlorobutyrate and 0.037 mL of DIPEA. The reaction was heated at 50 C. for 48 hours, then an additional 0.038 mL of methyl 4-chlorobutyrate, 0.074 mL of DIPEA and 3 mg of tetrabutylammonium iodide were added and heating continued at 70 C. for 48 hours. The reaction was evaporated under a stream of nitrogen and the residue purified by prep TLC (10% methanol in ethyl acetate) to give 41 mg of title compound and 17 mg of recovered starting material. Mass spec (ESI): 564 (M+1).

The chemical industry reduces the impact on the environment during synthesis Methyl 4-chlorobutyrate. I believe this compound will play a more active role in future production and life.

Reference:
Patent; Finke, Paul E.; Meurer, Laura C.; Mills, Sander G.; MacCoss, Malcolm; Qi, Hongbo; US2002/42431; (2002); A1;,
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Synthetic Route of 10203-58-4,Some common heterocyclic compound, 10203-58-4, name is Diethyl isobutylmalonate, molecular formula is C11H20O4, 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.

B. OCP-CO-CH(Bui)-CO2 Et Ethyl 2-(ethoxycarbonyl)-4-(methyl)pentanoate (6 g., 28 mM) was dissolved in ethanol (9 ml.) and 4 N-aqueous sodium hydroxide (7 ml.) was added. The mixture was stirred at ambient temperature for 1 hour and then evaporated. The residue was diluted with water (30 ml.) and the aqueous solution was washed with diethyl ether (3*10 ml.). The combined ethereal washings were backextracted with water (5 ml.). The combined aqueous phases were acidified to pH 3 at 0 C. with citric acid, and the resulting oil was extracted into ethyl acetate (4*20 ml.). The combined extracts were washed with water (2*20 ml.) and dried (MgSO4). The mixture was filtered and the solvent was evaporated to give 2-ethoxycarbonyl-4-methylpentanoic acid as an oil.

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

Reference:
Patent; Imperial Chemical Industries PLC; US4421744; (1983); A;,
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