Month: May 2021

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. 623-47-2, name is Ethyl propiolate, A new synthetic method of this compound is introduced below., HPLC of Formula: C5H6O2

a) (4-Chloro-phenyl)-propynoic acid ethyl esterA mixture of l-chloro-4-iodobenzene (120.4 g, 0.50 mol) and cesium carbonate (352.8 g, 1.0 mol) in tetrahydrofuran (1.275 L) was evaporated and flushed with argon. Then cuprous iodide (3.81 g, 20.0 mmol) and bis(triphenylphosphine)palladium(II) chloride (7.02 g, 10.0 mmol) were added and then ethyl propiolate (100 g, 1.01 mol) was added dropwise over a period of 20 min. The resulting dark brown suspension was stirred for 41 h at 35 C, then filtrated over Hyflo and washed with THF (5 L). The solution was concentrated and treated with toluene/heptane 1 :2 (1.5 L) and stirred for 1 h at 45 C under reduced pressure (250 mbar). The resulting suspension was filtered and the residue was washed with further toluene/heptane 1 :2 (1.5 L). The solid was dried affording 181.64 g (MS m/e: 209.0/211.2 [M+H]+) of a dark brown oil as crude product which was used 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:
Patent; F. HOFFMANN-LA ROCHE AG; KNUST, Henner; KOBLET, Andreas; NETTEKOVEN, Matthias; RATNI, Hasane; RIEMER, Claus; VIFIAN, Walter; WO2011/85886; (2011); A1;,
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Synthetic Route of 52787-14-1, A common heterocyclic compound, 52787-14-1, name is Methyl 4-(2-methoxy-2-oxoethyl)benzoate, molecular formula is C11H12O4, 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.

2- (4- (methoxycarbonyl) phenyl) acetic acid (58,24.04 dirty 1) to the reaction flask, 31111 water, 31111 5ml tetrahydrofuran and a mixed solvent of ethanol raw materials were dissolved. Was then added Eta0Eta-Eta20 (1.068,25.24pipiomicron1) alpha25 C was stirred for 10 hours the reaction is substantially complete. The solution was spin-off in tetrahydrofuran and ethanol, followed by addition of 26ml of dilute hydrochloric acid (lmmol / L), and a white precipitate formed, suction, infrared drying to give a white solid 4.4g, 94.4% yield

The synthetic route of 52787-14-1 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; China Pharmaceutical University; Xiang, Hua; Xu, Pei; Wang, Wenbin; Qian, Zhouyang; Chen, Mingqi; You, Qidong; (15 pag.)CN105541777; (2016); A;,
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Electric Literature of 2475-80-1,Some common heterocyclic compound, 2475-80-1, name is Methyl 2-amino-5-methoxybenzoate, molecular formula is C9H11NO3, 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) A solution of butyl lithium in hexane (2.5M, 18.5 ml) was added to a stirred solution of 1,5-dimethyl-tetrazole (4.55 g) in dry tetrahydrofuran (100 ml) at 0. After 30 minutes methyl 2-amino-5-methoxybenzoate (2.8 g) was added and stirring was continued for 3 hours. The reaction mixture was poured into water (200 ml), acidified with hydrochloric acid (5N) to pH 1, and extracted with dichloromethane (3*100 ml). The extract was dried over anhydrous magnesium sulphate and evaporated. The residue was recrystallized from industrial methylated spirit to give the novel compound 1-(2-amino-5-methoxyphenyl)-2-(1-methyl-1H-tetrazol-5-yl)ethanone, m.p. 170-172.

The synthetic route of 2475-80-1 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; The Boots Company Plc; US4659718; (1987); A;,
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Application of 150529-73-0,Some common heterocyclic compound, 150529-73-0, name is Methyl 2-(3-bromophenyl)acetate, molecular formula is C9H9BrO2, 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 dry 100 mL three-necked flask was added methyl 3-bromophenylacetate (4.58 g, 20 mmol, 1.0 eq) under N2.Add anhydrous tetrahydrofuran (30 mL),A 2.0 M solution of lithium diisopropylamide in THF / heptane / ethylbenzene (10.5 mL, 21 mmol, 1.05 eq) was slowly added dropwise at -78 C.After the completion of the dropwise addition, the mixture was stirred for 30 minutes, and then methyl iodide (2.84 g, 20 mmol,1.0eq). Stirring was continued at room temperature for a further 3 hours.60 mL of water was added to the reaction flask, followed by extraction with 50 mL of dichloromethane, and the mixture was separated.The aqueous phase was extracted twice more with 30 mL of dichloromethane. Combine the organic phase,Wash twice with saturated saline solution,Drying with anhydrous sodium sulfate, concentration, and the residue was separated by column chromatography.Methyl 2-(3-bromophenyl)propanoate 3.95 g was obtained in a yield of 82.3%.

The synthetic route of 150529-73-0 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Shenzhen Xianggen Biological Technology Co., Ltd.; Peng Jinan; Li Fanglin; Zhang Qishan; Luo Yuting; Xiao Qicai; Gao Liqian; (10 pag.)CN108794319; (2018); A;,
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These common heterocyclic compound, 37746-78-4, name is (E)-Ethyl 4-bromobut-2-enoate, 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: C6H9BrO2

General procedure: Amines 10a-f (1.0 equiv), N,N-diisopropylethylamine (1.5 equiv), ethyl (E)-4-bromobut-2-enoate(5, 1.3 equiv) and CH2Cl2 (25 mL) were placed in a round bottom flask and stirred at 20 C for1 h, under nitrogen. After completion of the reaction (TLC) the reaction mixture was extracted withNaHCO3 (3 30 mL) and water (1 30 mL). The organic phase was dried over Na2SO4 and thesolvent removed under reduced pressure to yield the crude product. The crude product was purifiedby silica gel column chromatography (9:1 hexanes:EtOAc).Ethyl (E)-4-(thiazolidin-3-yl)but-2-enoate (14a). 1.21 g (63 %) as a yellow oil.

The synthetic route of (E)-Ethyl 4-bromobut-2-enoate has been constantly updated, and we look forward to future research findings.

Reference:
Article; Rodriguez-Lozada, Josue; Tovar-Gudino, Erika; Guevara-Salazar, Juan Alberto; Razo-Hernandez, Rodrigo Said; Santiago, Angel; Pastor, Nina; Fernandez-Zertuche, Mario; Molecules; vol. 23; 11; (2018);,
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Reference of 6065-82-3, 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. 6065-82-3, name is Ethyl diethoxyacetate belongs to esters-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

To a mixture of boron trifluoride diethyl etherate (230 mL) in chloroform (640 mL) was added propane- 1,3 -dithiol (98.3 g, 0.91 mol) dropwise at -70 C. And then to the above solution was added ethyl 2,2- diethoxyacetate (160.0 g, 0.91 mol, in chloroform (160 mL)) dropwise at 70 C over 30 min. The resulting mixture was stirred at 70 C for 30 min. The reaction mixture was quenched by the addition of water (1500 mL), and the aqueous layer was extracted with DCM. The combined organic layer was washed with saturated sodium bicarbonate and brine, dried over anhydrous sodium sulfate and filtered. The filtrate was concentrated under vacuum. The residue was purified by flash column chromatography with 0-15% ethyl acetate in petroleum ether to afford ethyl l,3-dithiane-2-carboxylate (82.6 g, 47%) as a yellow oil.

The synthetic route of Ethyl diethoxyacetate has been constantly updated, and we look forward to future research findings.

Reference:
Patent; NURIX THERAPEUTICS, INC.; BARSANTI, Paul A.; BENCE, Neil F.; GOSLING, Jennifa; SAHA, Anjanabha; TAHERBHOY, Asad M.; ZAPF, Christoph W.; BOYLE, Kathleen; CARDOZO, Mario; MIHALIC, Jeffrey; LAWRENZ, Morgan; GALLOP, Mark; BRUFFEY, Jilliane; CUMMINS, Thomas; ROBBINS, Daniel; TANAKA, Hiroko; WANG, Chenbo; COHEN, Frederick; PALMER, Wylie; SANDS, Arthur T.; SHUNATONA, Hunter; (968 pag.)WO2019/148005; (2019); 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. 1014645-87-4, name is Methyl 4-(1-aminocyclopropyl)benzoate hydrochloride, A new synthetic method of this compound is introduced below., Quality Control of Methyl 4-(1-aminocyclopropyl)benzoate hydrochloride

Description 142: methyl 4-(1-(5-chloro-2-(2-phenylpyrrolidin-1- yl)nicotinamido)cyclopropyl)benzoate (D142)A solution of 5-chloro-2-(2-phenylpyrrolidin-1 -yl)nicotinic acid (D98) (150 mg, 0.5 mmol), methyl 4-(1 -aminocyclopropyl)benzoate hydrochloride (D7) (1 14 mg, 0.5 mmol) and N,N-Diisopropylethylamine (194 mg, 1 .5 mmol) in dimethylformamide (10ml) was stirred 1 h at room temperature, then benzotriazol-1 -yl- oxytripyrrolidinophosphonium hexafluorophosphate (PyBOP) (312 mg, 0.6 mmol) was added. The mixture was stirred at room temperature overnight, then poured into ice-water (20ml) and extracted with ethyl acetate (2x20ml). The organic solution was washed with brine (40ml), dried over Na2S04 and concentrated to obtain a residue which was purified by flash chromatography on silica gel eluting with a mixture petroleum ether/ethyl acetate (4:1 ). Collected fractions after solvent evaporation afforded the title compound (D142) (189 mg) as a yellow solid.1 H NMR (400MHz ,CHLOROFORM-d) delta (ppm): 8.10 (1 H, d, J = 2.4 Hz) 8.03 – 8.00 (2H, m) 7.74 (1 H, d, J = 2.4 Hz) 7.67 (1 H, s) 7.41 (2H, d, J = 8.0 Hz) 7.28 – 7.18 (5H, m) 5.36 – 5.32 (1 H, m) 3.91 (3H, s) 3.69 – 3.63 (1 H, m) 3.16 – 3.1 1 (1 H, m) 2.43 – 2.37 (1 H, m) 1 .97 – 1 .87 (3H, m) 1 .49 – 1 .39 (4H, m)

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; ROTTAPHARM S.P.A.; BORRIELLO, Manuela; ROVATI, Lucio; STASI, Luigi Piero; BUZZI, Benedetta; COLACE, Fabrizio; WO2012/76063; (2012); A1;,
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Adding a certain compound to certain chemical reactions, such as: 110482-96-7, name is Ethyl 2,2-difluoropent-4-enoate, 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 110482-96-7, Recommanded Product: Ethyl 2,2-difluoropent-4-enoate

PREPARATION 3 3,3-Difluoro-2-methyl-5-hexen-2-ol (Compound 4) To a solution of ethyl 2,2-difluoro-4-pentenoate (5.0 g, 30.5 mmol) in dry ether (50 ml) at -25 was added dropwise a solution of methyl magnesium bromide (3.0M; 30.5 ml). The mixture was stirred at -25 C. for half an hour and at 0 C. for 1 hour. The reaction mixture is poured into a saturated aqueous NH4 Cl solution (25 ml). The phases were separated and the aqueous phase was extracted with more ether (2*25 ml). The combined organic phases were dried with MgSO4 and concentrated. Flash chromatography (50 g silica gel, 5% ether in petroleum ether as eluant) to give the title compound as a colourless oil. NMR: delta=1.32 (t, 6H), 1.97 (bs, 1H), 2.74 (m, 2H), 5.20 (m, 2H), 5.92 (m, 1H) ppm.

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-difluoropent-4-enoate, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; Leo Pharmaceutical Products Ltd. A/S (L.o slashed.vens Kemiske Fabrik Produktionsaktieselskab); US5612325; (1997); A;,
Ester – Wikipedia,
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Adding a certain compound to certain chemical reactions, such as: 99974-66-0, name is Diethyl 3-hydroxycyclobutane-1,1-dicarboxylate, 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 99974-66-0, Quality Control of Diethyl 3-hydroxycyclobutane-1,1-dicarboxylate

Compound BB3-C (0.8 g, 0.0037 mol) was dissolved in dry DCM (16 mL) and cooled to 0 C. DAST (1.8 g, 0.011 mol) was added drop-wise to the cold solution. The reaction mixture was warmed to room temperature stirred for 12 h. The reaction mixture was quenched with cold saturated aHC03 solution. The crude product was extracted with DCM (100 mL). The organic layer was washed with 10 % NaHCOi solution, water followed by brine and dried over anhydrous Na2SO/t. Solvent was concentrated in vacuum and the crude product was purified by column chromatography (silica gel 60-120 mesh, eluent 1-2 % EtOAc in pet ether) which afforded the title compound as a pale yellow liquid (460 mg, yield 57 %). TLC system: 10% EtOAc in pet ether, Rf= 0.4.

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, Diethyl 3-hydroxycyclobutane-1,1-dicarboxylate, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; MEDIVIR UK LIMITED; AYESA, Susana; CARLQUIST, Peter; ERSMARK, Karolina; GRABOWSKA, Urszula; HEWITT, Ellen; JOeNSSON, Daniel; KAHNBERG, Pia; KLASSON, Bjoern; LIND, Peter; ODEN, Lourdes; PARKES, Kevin; WIKTELIUS, Daniel; WO2011/70541; (2011); A1;,
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Electric Literature of 23877-12-5, A common heterocyclic compound, 23877-12-5, name is tert-Butyl 2-bromo-2-methylpropanoate, molecular formula is C8H15BrO2, 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.

EXAMPLE III-2 tert-Butyl 2-(4-formylphenoxy)-2-methylpropanoate 24.42 g (200 mmol) of 4-hydroxybenzaldehyde are dissolved in 250 ml of N,N-dimethylformamide and treated with 27.64 g (200 mmol) of potassium carbonate. At 100 C., 53.55 g (240 mmol) of tert-butyl alpha-bromoisobutyrate are added dropwise. The mixture is stirred for another hour, a further 200 mmol of potassium carbonate and 240 mmol of tert-butyl alpha-bromoisobutyrate are added and, after 4 hours at 100 C., 1 l of water is added. Following extraction with diethyl ether, washing with 1 N aqeuous sodium hydroxide solution and saturated sodium chloride solution and drying over magnesium sulphate, the solvent is distilled off and the residue is purified by flash chromatography on silica gel (cyclohexane?cyclohexane/ethyl acetate 20:1?10:1?5:1) and dried under reduced pressure. The target compound is obtained in the form of colourless crystals in a yield of 42%. 1H-NMR (200 MHz, CDCl3): delta=1.40 (s, 9H), 1.62 (s, 6H), 6.91 (d, 2H), 7.79 (d, 2H), 9.88 (s, 1H). MS (ESI): 265 [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; Urbahns, Klaus; Woltering, Michael; Nikolic, Susanne; Pernerstorfer, Josef; Hinzen, Berthold; Dittrich-Wengenroth, Elke; Bischoff, Hilmar; Hirth-Dietrich, Claudia; Lustig, Klemens; US2003/32671; (2003); A1;,
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