Introduction of a new synthetic route about 4897-84-1

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 4897-84-1.

4897-84-1, Adding some certain compound to certain chemical reactions, such as: 4897-84-1, name is Methyl 4-bromobutanoate, 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 4897-84-1.

To a 250 mL flask equipped with a magnetic stirring bar, azepane, anhydrous acetonitrile (20 mL), methyl-4-bromobutyrate and potassium carbonate were added. A slight temperature increase was observed. The mixture was stirred at room temperature and the overall reaction time was 4 days. (0049) As the reaction proceeded, potassium carbonate was gradually consumed as it scavenged the liberated HBr to form potassium bromide (4.8 g) and potassium bicarbonate (4.0 g). (0050) DCM (10 mL) was added and the solid was collected by vacuum filtration. The organic phase was washed with deionized water (10 mL), separated, dried over MgSO4 and filtered, and the solvent was stripped using rotary evaporation. Yield: pale oil, 7.9 g, (>99percent). (0051) Characterization. FTIR: C?O, 1737, C?O, 1177 cm?1. (0052) H+ NMR: (CDCl3) delta ppm 3.67 (s, 3H), 2.61 (t, 4H), 2.48 (t, 2H), 2.34 (t, 2H), 1.77 (q, 2H), 1.62-1.58 (m, 8H).

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 4897-84-1.

Reference:
Patent; NOHMs Technologies, Inc.; Moganty, Surya; Abbate, Luigi; Torres, Gabriel; Brown, Kevin; Sinicropi, John; (13 pag.)US2017/305869; (2017); A1;,
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Sources of common compounds: Chloromethyl isopropyl carbonate

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35180-01-9, 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. 35180-01-9, name is Chloromethyl isopropyl carbonate, A new synthetic method of this compound is introduced below.

400 ml of ethanol, 50 ml of dimethylacetamide and 40 g of tenofovir monohydrate were added to a 1000 ml reaction flask,Stirring, control the temperature of 20 C dropwise add 85g of N, N-diisopropylethylamine, drop finished to continue dropping 100g chloromethyl carbonateThe reaction system was heated to 50 C for 8 hours and the monoester was detected to be less than 10%. The reaction solution was concentrated under 40 C under reduced pressure until no liquid flowed out and concentrated to the residue 500 ml of ethyl acetate, 200 ml of a 6% solution of sodium hydrogencarbonate,After stirring, the layers were extracted and the organic phase was washed twice with 200 ml of purified water,The obtained organic phase was dried over anhydrous sodium sulfate and concentrated to dryness under reduced pressure,The resulting concentrated residue was used directly in the next step.

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; Suzhou Homesun Pharmaceutical Co., Ltd.; Fan, chao; (7 pag.)CN105418683; (2016); A;,
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Brief introduction of 61367-07-5

The chemical industry reduces the impact on the environment during synthesis 61367-07-5. I believe this compound will play a more active role in future production and life.

The chemical industry reduces the impact on the environment during synthesis 61367-07-5, name is Methyl trans-4-aminocyclohexanecarboxylate hydrochloride, I believe this compound will play a more active role in future production and life. 61367-07-5

(1) Methyl trans-4-aminocyclohexanecarboxylate hydrochloride (47.5 g) obtained in Reference Example 2(1), bis(2-chloroethyl)ether (34.5 ml), sodium carbonate (77.9 g) and sodium iodide (88 g) are suspended in a mixture of tetrahydrofuran (1400 ml) and N,N-dimethylacetamide (280 ml). The mixture is then heated under reflux for 18 hours. Bis(2-chloroethyl)ether (23 ml) and sodium iodide (22 g) are added to the reaction solution and the mixture is refluxed for additional 6 hours. The reaction solution is concentrated under reduced pressure. The residue is dissolved in ethyl acetate/water and the organic layer is separated. The organic layer is washed with water and saturated brine, dried over sodium sulfate and evaporated to remove the solvent under reduced pressure. The resulting residue is purified by NH-silica gel column chromatography (eluent: ethyl acetate/hexane = 1/30, subsequently by ethyl acetate/hexane = 1/5 followed by 1/3) to give methyl trans-4-morpholin-4-ylcyclohexane-carboxylate (53.9 g). APCI-MS M/Z:228[M+H]+.

The chemical industry reduces the impact on the environment during synthesis 61367-07-5. I believe this compound will play a more active role in future production and life.

Reference:
Patent; TANABE SEIYAKU CO., LTD.; EP1582521; (2005); A1;,
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The origin of a common compound about 252881-74-6

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 252881-74-6.

252881-74-6, Adding some certain compound to certain chemical reactions, such as: 252881-74-6, name is tert-Butyl 3-(2-(2-(2-aminoethoxy)ethoxy)ethoxy)propanoate, 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 252881-74-6.

A solution of 2-14 (280 mg, 1.01 mmol), tert-butyl 3-(2-(2-(2-aminoethoxy)ethoxy) ethoxy)propanoate (2-15 where n=3, 337 mg, 1.22 mmol) and DIEA (0.7 mL, 4.04 mmol) in DMF (5 mL) was stirred at 80 C for overnight. The resulting mixture was diluted with EtOAc and washed with water five times. The organic layer was dried over Na2SO4, filtered, and concentrated under reduced pressure. The resulting residue was purified by flash column chromatography (DCM/EtOAc = 90 : 10 to 50 : 50) to afford 2-16 where n =3.

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 252881-74-6.

Reference:
Patent; DANA FARBER CANCER INSTITUTE, INC.; GRAY, Nathanael; JANG, Jaebong; DE CLERCQ, Dries; ECK, Michael; (201 pag.)WO2017/185036; (2017); A1;,
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Application of (E)-Ethyl 4-bromobut-2-enoate

At the same time, in my other blogs, there are other synthetic methods of this type of compound, (E)-Ethyl 4-bromobut-2-enoate, and friends who are interested can also refer to it.

As we all know, there are many different methods for the synthesis of a compound, and people can choose the synthesis method that suits their own laboratory according to the actual situation. 37746-78-4 name is (E)-Ethyl 4-bromobut-2-enoate, This compound is widely used in many fields, so it is necessary to find a new synthetic route. The downstream synthesis method of this compound is introduced below. 37746-78-4

General procedure: To a 50-mL round-bottomed flask were added ethyl pyrazole-5-carboxylate 1 (1.00 mmol), ethyl 4-bromobut-2-enoate 2 (2.00 mmol), potassium carbonate (0.28 g, 2.05 mmol) and C2H5OH (20 mL). The mixture was refluxed for 8 h. And then they were poured into water (100 mL) and extracted with CH2Cl2 (3 ¡Á 30 mL). The combined extracts were washed with water, dried over anhydrous Na2SO4 and filtered, and the solvent was removed by rotary evaporation. The crude products were purified by column chromatography to afford compounds 3a-f in 42-60%.

At the same time, in my other blogs, there are other synthetic methods of this type of compound, (E)-Ethyl 4-bromobut-2-enoate, and friends who are interested can also refer to it.

Reference:
Article; Yan, Peiling; Duan, Guiyun; Ji, Ruixue; Ge, Yanqing; Tetrahedron Letters; vol. 59; 25; (2018); p. 2426 – 2429;,
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Share a compound : Ethyl 3-bromobenzoate

At the same time, in my other blogs, there are other synthetic methods of this type of compound, 24398-88-7, and friends who are interested can also refer to it.

24398-88-7, 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 24398-88-7 as follows.

A mixture of 3- bromo-benzoic acid ethyl ester (229 mg, 1 mmol), 4-methylpiperidine ( 120 mg, 1 .2 mmol ), Pd2(dba)3 (25 mg ), BINAP (25 mg), and fBuONa ( 130 mg ) in toluene (6 mL) was heated at 90 C overnight. After the reaction was completed as indicated by TLC, the mixture was filtered and the filtrate was concentrated in vacuo. Ethyl acetate (50 mL) and aq. HC1 ( I , 20 mL) were then added. The aqueous portion was extracted with ethyl acetate (2 x 50 mL). The combined organic layers were washed with brine (50 mL), dried over anhydrous sodium sulfate, and filtered, concentrated, and purified by chromatography to give the title compound (76 mg, 3 1 %).

At the same time, in my other blogs, there are other synthetic methods of this type of compound, 24398-88-7, and friends who are interested can also refer to it.

Reference:
Patent; ARGUSINA INC.; LIAO, Jiayu; HONG, Yufeng; WANG, Yong; VON GELDERN, Thomas W.; ZHANG, Kanyin E.; WO2011/94890; (2011); A1;,
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Analyzing the synthesis route of 3-Fluorophenyl acetate

According to the analysis of related databases, 701-83-7, the application of this compound in the production field has become more and more popular.

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 701-83-7 as follows. 701-83-7

To 122 g (0.79 mol) of 3-fluorophenylacetate was added Aids (137 g, 1.03 mol) and theresulting mixture was heated at 160 C for 1.5 h then cooled at 0 C. HC1 IN was carefully addedfollowed by Et2O. The aqueous phase was extracted(2X) with Et2O and the combined organic phasewashed with brine, dried over Na2SO4 and evaporated to give the title compound.

According to the analysis of related databases, 701-83-7, the application of this compound in the production field has become more and more popular.

Reference:
Patent; MERCK FROSST CANADA & CO.; WO2004/108720; (2004); A1;,
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Brief introduction of 56525-63-4

Statistics shows that Methyl 3-chloro-4-methylbenzoate is playing an increasingly important role. we look forward to future research findings about 56525-63-4.

56525-63-4, Name is Methyl 3-chloro-4-methylbenzoate, 56525-63-4, 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.

(2-Chloro-4-(methoxycarbonyl)benzyl)triphenylphosphonium bromideMethyl 3-chloro-4-methylbenzoate (2.20 g, 11.96 mmol) was dissolved in carbon tetrachloride (30 mL) and N-bromosuccinimide (2.10 g, 11.80 mmol) was added followed by a catalytic amount of benzoyl peroxide (25 mg). The reaction mixture was refluxed for 6h. (ca. 90% conversion). After cooling to room temperature, a precipitate was filtered. The filtrate was concentrated to give crude brominated intermediate (3.20 g), which was used for the next step without further purification.

Statistics shows that Methyl 3-chloro-4-methylbenzoate is playing an increasingly important role. we look forward to future research findings about 56525-63-4.

Reference:
Patent; REPLIGEN CORPORATION; JACQUES, Vincent; RUSCHE, James R.; PEET, Norton P.; SINGH, Jasbir; WO2012/118782; (2012); A1;,
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Application of 369-26-6

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 369-26-6.

369-26-6, Adding some certain compound to certain chemical reactions, such as: 369-26-6, name is Methyl 3-amino-4-fluorobenzoate, 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 369-26-6.

To a solution of methyl 3-amino-4-fluorobenzoate (100 mg, 0.591 mmol) in DCM (3 ml) was added 4-(l-methylethyl)benzoyl chloride (162 mg, 0.887 mmol) and pyridine (96 mu, 1.18 mmol) at room temperature. The mixture was stirred for 1 h. 1 M HC1 and DCM were added and the phases were separated, the organic phase collected and the volatiles were removed in vacuo. The compound was purified by flash column chromatography. Yield: 135 mg (72percent); white solid. MS (ESI+) m/z 316 [M+H]+. HPLC purity: 99percent.

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 369-26-6.

Reference:
Patent; KANCERA AB; HAMMER, Kristin; JOeNSSON, Mattias; KRUeGER, Lars; (230 pag.)WO2017/108282; (2017); A1;,
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Application of Methyl 4-bromobenzoate

According to the analysis of related databases, 619-42-1, the application of this compound in the production field has become more and more popular.

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 619-42-1 as follows. 619-42-1

Synthesis methyl 4-(phenylamino)benzoate (Compound 17) Under argon atmosphere, a solution of methyl 4-bromobenzoate (3.5 g, 16.28 mmol), aniline (1.819 g, 19.53 mmol), palladium (II) acetate (218 mg, 0.97 mmol), rac-BINAP (506 mg, 0.81 mmol), and potassium carbonate (6.72 g, 48.62 mmol) in toluene (ca. 10 mL) was tightly capped in a 25 mL microwave vessel. The mixture was subjected to microwave irradiation at 160 C. for 2 h and then cooled to room temperature. The reaction mixture was diluted with DCM and filtered. The organic solvents were evaporated in vacuo, and the residue was suspended in methyl tert-butyl ether (150 mL). The organic phase was washed with saturated aqueous sodium bicarbonate, brine, dried (MgSO4), filtered and evaporated in vacuo. The obtained residue was purified by column chromatography (5% EtOAc in heptane to 60% EtOAc in heptane) to afford title compound 6 (3.55 g, 96% yield) as a pale green solid: mp 121-122 C.

According to the analysis of related databases, 619-42-1, the application of this compound in the production field has become more and more popular.

Reference:
Patent; Diaz, Philippe; Diaz, Fanny; Petrov, Ravil Rashitovich; US2012/39804; (2012); A1;,
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Ester – an overview | ScienceDirect Topics