Month: May 2021

Application of 3618-04-0, 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. 3618-04-0 name is trans-Ethyl 4-hydroxycyclohexanecarboxylate, 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.

Example 7: c/s-4-hydroxy-4- [2-(6-methoxy- [1,5] naphthyridin-4-yl)-ethyl] – cyclohexanecarboxylic acid (2,3-dihydro-benzo[l,4]dioxin-6-yl)-amide:7.i. 4-oxo-cyclohexanecarboxylic acid ethyl ester.To a solution of oxalyl chloride (6 mL, 68.8 mmol) in DCM (100 mL) at -78C was added dropwise a solution of DMSO (6.4 mL, 90 mmol) in DCM (2O mL). The mixture was stirred at this temperature for 15 min before the dropwise addition of a solution of ethyl4-hydroxycyclohexane carboxylate (4.8 mL, 30 mmol) in DCM (20 mL). The mixture was stirred at -78C for 3 h before addition of TEA (29.3 mL, 210 mmol) in DCM (20 mL).The mixture was then gradually warmed to rt, washed with a sat. aq. NH4Cl solution and brine, dried over MgSO4 and concentrated. The residue was purified by chromatography over SiO2 (Hex/EA 1 :1) to give the title ketone (4.6 g, 90% yield) as a colourless oil.1H NMR (CDCl3) delta: 4.19 (q, J = 7.1 Hz, 2H); 2.80-2.70 (m, IH); 2.55-2.45 (m, 2H);2.40-2.30 (m, 2H); 2.25-2.10 (m, 2H); 2.05-2.00 (m, 2H); 1.29 (t, J = 7.1 Hz, 3H).

At the same time, in my other blogs, there are other synthetic methods of this type of compound, trans-Ethyl 4-hydroxycyclohexanecarboxylate, and friends who are interested can also refer to it.

Reference:
Patent; ACTELION PHARMACEUTICALS LTD; WO2007/107965; (2007); A1;,
Ester – Wikipedia,
Ester – an overview | ScienceDirect Topics

Related Products of 3618-04-0, 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. 3618-04-0, name is trans-Ethyl 4-hydroxycyclohexanecarboxylate, This compound has unique chemical properties. The synthetic route is as follows.

Step (i) 4-Toluenesulfonyl chloride (18.29 g, 96 mmol) was added in several portions to a solution of ethyl 4-hydroxycyclohexanecarboxylate (ca. 1 : 1 mixture of cis and trans ring isomers) (29.5 g, 90 mmol) in pyridine (100 niL) in an ice-water bath, and the mixture stirred, allowing to warm to RT. After the solid had dissolved, the mixture was allowed to stand. After 24 h, the mixture was concentrated and the residue partitioned between water and EtOAc (100 ml. each). The organic phase was dried and concentrated to give ethyl 4- (tosyloxy)cyclohexanecarboxylate (ca. 1 : 1 mixture of cis and trans ring isomers) (crude, 29.5 g) as a colourless oil which was used in the next step without further purification. NMR (400 MHz, CDC13) delta ppm 1.20-1.30 (m, 3H) 1 .44-2.08 (m, 81 ) 2.2 1 -2.43 (m, 111 ) 2.48 (s, 31 1) 4.08-4.20 (m, 211 ) 4.40-4.50 and 4.70-4.78 (both m, total 1H) 7.28-7.40 (m, 2H) 7.78-7.86 (m, 2H)

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

Reference:
Patent; TAKEDA PHARMACEUTICAL COMPANY LIMITED; TAKEDA CAMBRIDGE LIMITED; BUFFHAM, William; CANNING, Hannah; DAVENPORT, Richard; FARNABY, William; MACK, Stephen; PARMAR, Alka; WRIGHT, Susanne; WO2015/25164; (2015); A1;,
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. 711-01-3, name is Methyl adamantane-1-carboxylate belongs to esters-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below. name: Methyl adamantane-1-carboxylate

To 97 g (499 mmol) of methyl 1-adamantanecarboxylate obtained in Preparation Example 1, 485 g of toluene was added, and nitrogen substitution was carried out, followed by cooling with a refrigerant.While maintaining the toluene solution at 10 ¡ã C. or less, 270 mL (540 mmol) of a solution of methylmagnesium chloride in tetrahydrofuran (THF) (2 M) is added dropwiseThereafter, the temperature was raised naturally, and reaction was performed at room temperature (25 ¡ã C.) for 3 hours.The reaction solution was cooled again with a refrigerant, and 179 g (1160 mmol) of methacrylic anhydride was added dropwise while maintaining the temperature at 10 ¡ã C. or less.Thereafter, the temperature was raised naturally, and reaction was performed at room temperature (25 ¡ã C.) for 3 hours.The crude reaction solution was washed with a 2N aqueous hydrochloric acid solution while keeping the temperature at 25 ¡ã C. or lower, and the aqueous layer was separated.Subsequently, the organic layer obtained is washed with a 10percent aqueous sodium hydroxide solution and saturated brine, and the solvent is evaporated under reduced pressure,Crude 1- (1-adamantyl) -1-methylethyl methacrylate was obtained.(Yield 129.9 g, GC purity 82.3percent)

The synthetic route of 711-01-3 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Osaka Organic Chemical Industry Ltd.; Kojima, Akio; Kono, Naoya; Uenoyama, Yoshitaka; (20 pag.)JP6478447; (2019); B2;,
Ester – Wikipedia,
Ester – an overview | ScienceDirect Topics

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. 4131-74-2, name is Dimethyl 3,3-Thiodipropionate, A new synthetic method of this compound is introduced below., Recommanded Product: Dimethyl 3,3-Thiodipropionate

Preparation example 1: Methyl 4-oxotetrahydrothiopyrane-3-carboxylate A solution (100 ml) of dimethyl 3,3′-thiodipropionate (8.25 g) in anhydrous tetrahydrofuran was added with sodium hydride (2.11 g) and heated under reflux for 5 hours. The reaction mixture was cooled, then added with acetic acid (8 ml), poured into water, and extracted with ether. The organic layer was dried over anhydrous magnesium sulfate and then evaporated under reduced pressure to obtain the above-titled product.

The synthetic route of 4131-74-2 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Meiji Seika Kaisha, Ltd.; EP1142881; (2001); A1;,
Ester – Wikipedia,
Ester – an overview | ScienceDirect Topics

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. 13380-85-3, name is Methyl 4-(hydroxymethyl)cyclohexanecarboxylate, A new synthetic method of this compound is introduced below., HPLC of Formula: C9H16O3

The compound represented by Formula (1-1-2), pyridine, anddichloromethane were put into a reaction container under a nitrogen atmosphere. With ice cooling, methanesulfonyl chloride wasdropped, followed by stirring at room temperature. After ordinary post-treatment was performed, purification was performed by column chromatography (silica gel) to obtain a compound represented by Formula (1-1-3).

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; DIC CORPORATION; TENG, Yan; HORIGUCHI, Masahiro; KADOMOTO, Yutaka; KOISO, Akihiro; HAYASHI, Masanao; SAITOU, Yoshitaka; LI, Zhimin; (201 pag.)WO2017/79867; (2017); A1;,
Ester – Wikipedia,
Ester – an overview | ScienceDirect Topics

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. 251458-15-8, name is Methyl 2-(3-bromophenyl)-2-methylpropanoate, A new synthetic method of this compound is introduced below., COA of Formula: C11H13BrO2

To a solution of ester from step 1 in THF-MeOH (4: 1,0. 5M) was added LIOH (3 eq, 2M) and the mixture was stirred at 50C for 1h. The organic solvent evaporated, aqueous was acidified with HCl IN and the acid extracted with EtOAc (3X). The organic was washed with brine, dried and solvent evaporated to afford the acid.

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; MERCK FROSST CANADA & CO.; WO2004/48374; (2004); A1;,
Ester – Wikipedia,
Ester – an overview | ScienceDirect Topics

Reference of 56441-97-5, 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. 56441-97-5, name is Methyl 4-(benzyloxy)-3-methoxybenzoate belongs to esters-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

REFERENCE EXAMPLE 15 Methyl 5-methoxy-2-nitro-4-(benzyloxy) benzoate Nitric acid (27 mL of a 70% solution) was added dropwise to a suspension of methyl 3-methoxy-4-(benzyloxy) benzoate (14.5 g, 53.0 mmol) in 150 mL of acetic acid. The mixture was stirred at room temperature for 15 minutes and then was heated at 50 C. for 4 hours. The reaction was cooled to room temperature and poured into ice. The precipitate was collected by filtration, washed with water and dried to provide 16.4 g of methyl 5-methoxy-2-nitro-4-(benzyloxy) benzoate as an off-white solid, mp 104-105 C.; MS (ES) m/z 318.1 (M+1). Analysis for C16H15NO6: Calcd: C, 60.57;H, 4.76; N, 4.41. Found: C, 60.39;H, 4.70; N, 4.28.

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-(benzyloxy)-3-methoxybenzoate, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; American Home Products Corporation; US2002/26052; (2002); A1;,
Ester – Wikipedia,
Ester – an overview | ScienceDirect Topics

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. 72338-48-8, name is Ethyl 12-bromododecanoate, This compound has unique chemical properties. The synthetic route is as follows., COA of Formula: C14H27BrO2

c) Synthesis of ethyl 13-(diethoxyphosphoryl)tridecanoate In a single-neck flask with a reflux condenser, ethyl 12-bromododecanoate is weighed (1.8 g, 7.37 mmol) and triethyl phosphite (2.6 mL, 15 mmol) is added. The reaction mixture is brought to 150C and left stirring under a static head of nitrogen. After 24 hours the one neck balloon is attached to the high vacuum pump to eliminate volatile products and the resulting dense oil is directly loaded with column chromatography on silica gel. It is eluted with a mixture of ethyl acetate/petroleum ether 1/1 which leads to the isolation of 2.5 g (yield 94%) of ethyl 13-(diethoxyphosphoryl)tridecanoate as a colourless oil.

According to the analysis of related databases, 72338-48-8, the application of this compound in the production field has become more and more popular.

Reference:
Patent; Colorobbia Italia S.p.a.; EP1979365; (2012); B1;,
Ester – Wikipedia,
Ester – an overview | ScienceDirect Topics

Application of 927-68-4, The chemical industry reduces the impact on the environment during synthesis 927-68-4, name is 2-Bromoethyl acetate, I believe this compound will play a more active role in future production and life.

Step 14b. 2-(6-Amino-8-(6-iodobenzo[d][1,3]dioxol-5-ylthio)-9H-purin-9-yl)ethyl acetate (Compound 401-38); A mixture of compound 105-38 (3.89 g, 9.41 mmol), Cs2CO3 (3.68 g, 11.3 mmol), 2-bromoethyl acetate (1.89 g, 11.3 mmol) and anhydrous DMF (50 mL) was stirred for 2 h at 50 C. The solvent was removed under high vacuum and the crude purified by column chromatography on silica gel (CH2Cl2/MeOH=60/1) to provide target compound 401-38 as a pale yellow solid (2.95 g, 62.8%): LCMS: 500 [M+1]+.

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, 2-Bromoethyl acetate, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; Qian, Changgeng; Cai, Xiong; Gould, Stephen; Zhai, Haixiao; US2008/234297; (2008); A1;,
Ester – Wikipedia,
Ester – an overview | ScienceDirect Topics

Synthetic Route of 369-26-6, These common heterocyclic compound, 369-26-6, name is Methyl 3-amino-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.

HATU (116 mg, 0.305 mmol) was added to picolinic acid (37.5 mg, 0.305 mmol) and DIPEA (66 mu, 0.381 mmol) in DMF (2 ml). After 15 min, methyl 3-amino-4-fluorobenzoate (43 mg, 0.254 mmol) in DMF (1 ml) was added. The mixture was stirred at ambient temperature for 10 d before solvent was evaporated and residue dissolved in EtOAc. The solution was washed with sat. NaHC03, dried (MgS04) and evaporated. Half of the crude material from above (0.127 mmol) was dissolved in dioxane (1.5 ml) and MeCN (1.5 ml). Potassium carbonate (35 mg, 0.254 mmol) was added and the mixture was heated at 180 ¡ãC for 2 h in a microwave reactor. Silica gel was added and solvents evaporated. The dry silica was applied on a flash column which was eluted with 35-50percent) EtOAc in hexanes. Yield: 6 mg (18percent>); colourless oil.

Statistics shows that Methyl 3-amino-4-fluorobenzoate is playing an increasingly important role. we look forward to future research findings about 369-26-6.

Reference:
Patent; KANCERA AB; HAMMER, Kristin; JOeNSSON, Mattias; KRUeGER, Lars; (230 pag.)WO2017/108282; (2017); A1;,
Ester – Wikipedia,
Ester – an overview | ScienceDirect Topics