Tag: M.W=300-400

Adding a certain compound to certain chemical reactions, such as: 581065-95-4, name is tert-Butyl 1-amino-3,6,9,12-tetraoxapentadecan-15-oate, 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 581065-95-4, name: tert-Butyl 1-amino-3,6,9,12-tetraoxapentadecan-15-oate

[00225j Synthesis of N- [(PEG)4C00-t-Buj -N?-Boc-N?-methyl-ethylenediamine .To the solution of N-t-BuOOC-(PEG)4-amine (0.557g , 1.73 mmol) in 20 ml of methanol, (N-methyl)N-Boc acetaldehyde (0.3 g, 1.73 mmol) was added. The mixture was stirred at room temperature for 3 hours. NaBH4 (0.196g, 5.2 mmol) was added to the mixture at 0C, and the resultant mixture was stirred at 0C for 1 hour and 1 hour at room temperature. The reaction was quenched by adding 5 ml of water. After removal of solvent, 5 ml of water was added, and the mixture was extracted three times with methylene chloride. The combined organic layer was dried over Na2SO4, and the product was purified by flash silica chromatography using heptane/ethyl acetate to methylene chloride/methanol to give a yield of 64.5% (0.535 g). ?H NMR (300 MHz, CD2C12) 3 ppm: 3.5-3.8 (m, 18H, CH2), 3.45 (br, 2H, CH2), 2.98 (br, 2H, CH2), 2.83 (s, 3H, NCH3), 2.46 (t, 2H, COCH2), 1.42 (s, 18H, CH3); MS-ESI (mle): 479.6 [M+H].

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; PROMEGA CORPORATION; MUSTAFA, Dana; ZHOU, Wenhui; MEISENHERMIER, Poncho; DUELLMAN, Sarah; MA, Dongping; CALI, James, J.; WO2015/116867; (2015); A1;,
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Reference of 18013-97-3, 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. 18013-97-3 name is Diethyl 2,5-dibromoterephthalate, 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.

To a 100 mL dry three-necked flask with a magnetic rotor and a condenser, diethyl 2,5-dibromo-terephthalate (3.80 g, 10.0 mmol, 1.0 eq) was added sequentially.Phenylboronic acid (1.21 g, 10.0 mmol, 1.0 eq), tetrakis(triphenylphosphine)palladium (Pd(PPh3)4) (570 mg, 0.5 mmol, 0.05 eq),Na2CO3 (2.12 g, 20 mmol, 2.0 eq).Nitrogen gas was distilled three times, then toluene (60.0 mL) and ethanol (20.0 mL) were added.Nitrogen gas was then bubbled for 20 minutes and the mixture was placed in a 90 C oil bath for 36 hours.The mixture was cooled to room temperature, and the solvent was evaporated under reduced pressure.Eluent (petroleum ether / dichloromethane = 3: 1-1: 1) to give 3 as a white solid 256 mg, 7% yield.

At the same time, in my other blogs, there are other synthetic methods of this type of compound, Diethyl 2,5-dibromoterephthalate, and friends who are interested can also refer to it.

Reference:
Patent; Zhejiang University of Technology; Ruisheng Optoelectric Science And Technology (Changzhou) Co., Ltd.; Li Guijie; Lou Weiwei; Huang Da; Chen Shaohai; (46 pag.)CN109678906; (2019); A;,
Ester – Wikipedia,
Ester – an overview | ScienceDirect Topics

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. 179688-27-8, name is Ethyl 2-amino-4,5-bis(2-methoxyethoxy)benzoate belongs to esters-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below. Recommanded Product: Ethyl 2-amino-4,5-bis(2-methoxyethoxy)benzoate

In a 10-mL volume stainless steel pressure-resistant vessel were placed 1.02 g (3.3 mmol) of ethyl 4,5-bis(2-methoxyethoxy)anthranilate, 0.96 g (9.1 mmol) of methyl orthoformate, 0.69 g (9.1 mmol) of ammonium acetate, and 5.0 mL of methanol. The reaction was carried out at 110C for 6 hours. After the reaction was complete, the reaction mixture was cooled to room temperature and concentrated under reduced pressure. Then, the concentrate was recrystallized from 20 mL of methanol. The crystalline product was collected by filtration and dried under reduced pressure to give 0.87 g (isolated yield: 91%) of 6,7-bis(2-methoxyethoxy)quinazolin-4-one as a white crystalline product.

The synthetic route of 179688-27-8 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Ube Industries, Ltd.; EP1477481; (2004); A1;,
Ester – Wikipedia,
Ester – an overview | ScienceDirect Topics

Reference of 18014-00-1, 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 18014-00-1 as follows.

General procedure: To a 15 mL vial tube equipped with a magnetic stirring bar and a teflon screw cap were addeddimethyl 2,5-dibromoterephthalate (0.28 g, 0.8 mmol),1) N-methylaniline derivative (8.0 mmol),Pd2(dba)3 (34 mg, 0.06 mmol), RuPhos (70 mg, 0.24 mmol), K3PO4 (1.70 g, 8.0 mmol), and toluene(3.2 mL) under argon atmosphere. The mixture was stirred at 100 C for 10 h. The resultingmixture was allowed to cool to room temperature, and CH2Cl2 (10 mL) was added to the vial. Theprecipitate was removed by suction filtration and the filtrate was concentrated by evaporation underreduced pressure. The crude product was purified by column chromatography on silica gel(hexane/CH2Cl2 2:1 to 1:1) to give 1.

According to the analysis of related databases, 18014-00-1, the application of this compound in the production field has become more and more popular.

Reference:
Article; Shimizu, Masaki; Asai, Yuiga; Takeda, Youhei; Yamatani, Akinori; Hiyama, Tamejiro; Tetrahedron Letters; vol. 52; 32; (2011); p. 4084 – 4089;,
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Electric Literature of 764667-64-3,Some common heterocyclic compound, 764667-64-3, name is 5-(1-Hydroxy-2-(2,4,5-trifluorophenyl)ethylidene)-2,2-dimethyl-1,3-dioxane-4,6-dione, molecular formula is C14H11F3O5, 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.

547 gm of 4-oxo-4-[3-(trifiuoromethyl)-556-dihydro[l,2,4]triazolo[4,3-alpha]pyrazin-7(8H)- yl]-l-(2,4,5-trifiuororhohenyl)butan-2-one (Formula V) was obtained by adding 500 gm of 5-[l-hydroxy-2-(2,4,5-trifluorophehy)ethylidene]-2,2-dimethyl-l ,3-dioxane-4,6- dione in to the solution 5000 ml toluene containing 440 gm of ‘ 3-(trifluoromethyl)-5,6,7,8-tetrahydro[l,2,4]triazolo[4,3-?]pyrazine .hydrochloride (Formula VI) and 1100 ml of diisopropyl ethylamine at 25-3O0C followed by heating the reaction mass to toluene reflux temperature till the completion of reaction monitor by TLC or HPLC. Isolation of the above said product done by’, ethylacetate and. aqueous -acidic workup followed by distillation.The isolated compound has been characterized by, Mass and HPLC purity. Mass : 407.18 [M+H]+HPLC purity ‘ . : NLT – 85 %. ‘ ‘ ‘ i

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 5-(1-Hydroxy-2-(2,4,5-trifluorophenyl)ethylidene)-2,2-dimethyl-1,3-dioxane-4,6-dione, its application will become more common.

Reference:
Patent; GLENMARK GENERICS LIMITED; WO2009/84024; (2009); A2;,
Ester – Wikipedia,
Ester – an overview | ScienceDirect Topics

Synthetic Route of 764667-64-3, 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. 764667-64-3, name is 5-(1-Hydroxy-2-(2,4,5-trifluorophenyl)ethylidene)-2,2-dimethyl-1,3-dioxane-4,6-dione, This compound has unique chemical properties. The synthetic route is as follows.

A round bottom flask is charged with 3-trifluoromethyl-5,6,7,8-tetrahydro- 1 ,2,4-thazolo[4,3a]pyrazine hydrochloride (144.6 g) and ethyl acetate (2000 ml_) at 28C, then N-methylmorpholine (67.2 g) is added. 5-[1 -hydroxy-2-(2,4,5- trifluorophenyl)ethyledine]-2,2-dimethyl-1 ,3 dioxane-4,6-dione (200 g) is added and the mixture is heated to reflux for 6 hours. The mixture is slowly cooled to room temperature. Water (1000 ml_) is added, the mixture is stirred for 15 minutes, and the organic layer is separated. The aqueous layer is extracted with ethyl acetate (200 ml_). The two organic layers are combined and solvent is distilled at 37C. Toluene (400 ml_) is added to the residue and stirred for 3 hours. The solid is filtered, washed with toluene (200 ml_), and dried under reduced pressure at 500C for 12.5 hours, to afford the title compound. (252.0 g, 98.1 % yield).

The chemical industry reduces the impact on the environment during synthesis 5-(1-Hydroxy-2-(2,4,5-trifluorophenyl)ethylidene)-2,2-dimethyl-1,3-dioxane-4,6-dione. I believe this compound will play a more active role in future production and life.

Reference:
Patent; DR. REDDY’S LABORATORIES LTD.; DR. REDDY’S LABORATORIES, INC.; BANDICHHOR, Rakeshwar; GUDIMALLA, Nagaraju; DWIVEDI, Namrata; CHETLURU, Kiran Kumar; GADE, Srinivas Reddy; MUVVA, Venkateswarlu; SRIVASTAVA, Bindu; WO2011/25932; (2011); A2;,
Ester – Wikipedia,
Ester – an overview | ScienceDirect Topics

Synthetic Route of 764667-64-3, 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. 764667-64-3, name is 5-(1-Hydroxy-2-(2,4,5-trifluorophenyl)ethylidene)-2,2-dimethyl-1,3-dioxane-4,6-dione, This compound has unique chemical properties. The synthetic route is as follows.

A round bottom flask is charged with 3-trifluoromethyl-5,6,7,8-tetrahydro- 1 ,2,4-thazolo[4,3a]pyrazine hydrochloride (144.6 g) and ethyl acetate (2000 ml_) at 28C, then N-methylmorpholine (67.2 g) is added. 5-[1 -hydroxy-2-(2,4,5- trifluorophenyl)ethyledine]-2,2-dimethyl-1 ,3 dioxane-4,6-dione (200 g) is added and the mixture is heated to reflux for 6 hours. The mixture is slowly cooled to room temperature. Water (1000 ml_) is added, the mixture is stirred for 15 minutes, and the organic layer is separated. The aqueous layer is extracted with ethyl acetate (200 ml_). The two organic layers are combined and solvent is distilled at 37C. Toluene (400 ml_) is added to the residue and stirred for 3 hours. The solid is filtered, washed with toluene (200 ml_), and dried under reduced pressure at 500C for 12.5 hours, to afford the title compound. (252.0 g, 98.1 % yield).

The chemical industry reduces the impact on the environment during synthesis 5-(1-Hydroxy-2-(2,4,5-trifluorophenyl)ethylidene)-2,2-dimethyl-1,3-dioxane-4,6-dione. I believe this compound will play a more active role in future production and life.

Reference:
Patent; DR. REDDY’S LABORATORIES LTD.; DR. REDDY’S LABORATORIES, INC.; BANDICHHOR, Rakeshwar; GUDIMALLA, Nagaraju; DWIVEDI, Namrata; CHETLURU, Kiran Kumar; GADE, Srinivas Reddy; MUVVA, Venkateswarlu; SRIVASTAVA, Bindu; WO2011/25932; (2011); A2;,
Ester – Wikipedia,
Ester – an overview | ScienceDirect Topics

Adding a certain compound to certain chemical reactions, such as: 111-61-5, name is Ethyl stearate, 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 111-61-5, Quality Control of Ethyl stearate

Reaction experiments were carried out in a 50 ml stainless steelautoclave. All the catalysts were pre-reduced in hydrogen at tem-perature (150, 200, 500C) for 90 min before the reaction. Afterreduction, the catalyst was transferred into the autoclave, in which5.0 ml hexane was added as solvent, under the protection of hydro-gen. After that, a certain amount of ethyl stearate was added andthe autoclave was sealed. The reaction was operated under a stir-ring rate of 1300 rpm (without diffusion limitation) at 230C and aH2pressure of 3.0 MPa H2. After the reaction for several hours, the autoclave was cooled to room temperature. The products were col-lected and then analyzed by gas chromatography with FID detectorwith a DB-1 capillary column and GC-MS.

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

Reference:
Article; He, Limin; Li, Xiaoru; Lin, Weiwei; Li, Wei; Cheng, Haiyang; Yu, Yancun; Fujita, Shin-Ichiro; Arai, Masahiko; Zhao, Fengyu; Journal of Molecular Catalysis A: Chemical; vol. 392; (2014); p. 143 – 149;,
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Ester – an overview | ScienceDirect Topics

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 869-10-3 as follows. Computed Properties of C10H16Br2O4

To a solution of diethyl 2,5-dibromoadipate (36 g, 100 mmol) in N, N-dimethylformamide (150 mL) was added sodium sulfide (11.8 g, 150 mmol) at room temperature and stirred at room temperature 5 hours.Water and ethyl acetate were added to the reaction, the organic phase was separated, washed with saturated brine, dried and concentrated, and then separated by column chromatography (ethyl acetate / petroleum ether = 1/20) to give the title compound (11.6 g, 50%).

According to the analysis of related databases, 869-10-3, the application of this compound in the production field has become more and more popular.

Reference:
Patent; Beijing Sai Lintai Pharmaceutical Co., Ltd.; Liang Zhi; Liu Zhihua; Dai Yusen; Hu Yuandong; Sun Ying; Huang Yuanyuan; Peng Yong; Kong Fansheng; Luo Hong; Han Yongxin; (76 pag.)CN107474024; (2017); A;,
Ester – Wikipedia,
Ester – an overview | ScienceDirect Topics

Synthetic Route of 205448-64-2, The chemical industry reduces the impact on the environment during synthesis 205448-64-2, name is Methyl 4-(((2,2-dimethyl-4,6-dioxo-1,3-dioxan-5-ylidene)methyl)amino)-2-methoxybenzoate, I believe this compound will play a more active role in future production and life.

5-((3-Methoxy-4-methoxycarbonylanilino)methylene)-2,2-dimethyl-1,3-dioxane-4,6-dione (10 g, 29.8 mmol) was suspended in DOWTHERM A, (trade mark of Fluka Chemie AG), (125 ml) and heated to 180-190 C. over 30 minutes.. The starting material dissolved at 100 C. and carbon dioxide came off at approximately 180 C. The heating was stopped after a further 30 minutes and the product precipitated out as the temperature dropped.. Upon reaching 40 C. ether was added and the mixture was stirred for 30 minutes.. The solid was collected by filtration, washed with ether and dried under vacuum to give 7-methoxy-6-methoxycarbonyl-1,4-dihydroquinolin-4-one (5.56 g, 80%). 11H NMR Spectrum: (DMSOd6) 3.80 (s, 3H); 3.85 (s, 3H); 5.95 (d, 1H); 7.00 (s, 1H); 7.85 (d, 1H); 8.40 (s, 1H); 11.6 (br s, 1H); MS-ESI: 234 [MH]+;

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-(((2,2-dimethyl-4,6-dioxo-1,3-dioxan-5-ylidene)methyl)amino)-2-methoxybenzoate, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; Zeneca Limited; Zeneca Pharma S.A.; US6809097; (2004); B1;,
Ester – Wikipedia,
Ester – an overview | ScienceDirect Topics