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9/1/2021 News Some tips on 3044-06-2

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 2-(1-ethoxyethylidene)malonate, other downstream synthetic routes, hurry up and to see.

Synthetic Route of 3044-06-2, The chemical industry reduces the impact on the environment during synthesis 3044-06-2, name is Diethyl 2-(1-ethoxyethylidene)malonate, I believe this compound will play a more active role in future production and life.

General procedure: Diethyl ethoxymethylenemalonate (4.6mmol) were add to a solution of sodium hydride (9.7mmol) and compound 14a-l (4.2mmol) in ethanol (20mL), the reaction mixture was stirred at 80C for 2h. After the reaction completed, the mixture was added 10mL 6M hydrochloric acid and stirred for 0.5h, then the precipitate was collected by filtration. The resulting residue was recrystallized from ethanol to yield ethyl 2-(4-alkoxyphenyl-3-cyano)-6-oxo-1,6-dihydropyrimidine-5-carboxylate(15a-l).

Reference:
Article; Mao, Qing; Dai; Xu, Gaoyang; Su, Yu; Zhang, Bing; Liu, Dan; Wang, Shaojie; European Journal of Medicinal Chemistry; vol. 181; (2019);,
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A new synthetic route of Diethyl 2-(1-ethoxyethylidene)malonate

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. 3044-06-2, name is Diethyl 2-(1-ethoxyethylidene)malonate, A new synthetic method of this compound is introduced below., name: Diethyl 2-(1-ethoxyethylidene)malonate

4-isopropoxy-3-cyanobenzidine hydrochloride (1 g, 0.0042 mol), M-230 (1.06 g, 0.0046 mol),A fresh methanol solution of sodium ethoxide (3 g of sodium hydride (20%) was added to 100 ml of ethanol at a low temperature) (20 ml), and refluxed for 2 hours. After the reaction was completed by TLC, the reaction mixture was cooled to room temperature, and 6N was gradually added to the reaction mixture. ofThe pH of the mixture was adjusted to 1 with HCl, stirred for 30 min, filtered, filtered, washed with water and dried. The obtained crude product was recrystallized from ethanol to give a white solid, 0.44 g.Yield: 31.1%

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; Shenyang Hainuowei Pharmaceutical Technology Co., Ltd.; Wang Shaojie; Mao Qing; Zhang Bing; (30 pag.)CN110156698; (2019); A;,
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Sources of common compounds: Diethyl 2-(1-ethoxyethylidene)malonate

These common heterocyclic compound, 3044-06-2, name is Diethyl 2-(1-ethoxyethylidene)malonate, 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. Application In Synthesis of Diethyl 2-(1-ethoxyethylidene)malonate

Reference Example 196 Ethyl 4-hydroxy-6-methylpyrimidine-5-carboxylate A mixture of diethyl malonate (4.8 mL), triethyl orthoacetate (17 mL), acetic anhydride (0.11 mL) and zinc chloride (1.2 g) was stirred at 140C. To the mixture was added acetic anhydride (0.11 mL) each after 30, 90 and 120 minutes, and then stirred at the same temperature overnight. The reaction mixture was cooled to room temperature, and the insoluble material was removed by filtration. The filtrate was concentrated under reduced pressure, and the residue was purified by column chromatography on silica gel (eluent: n-hexane/ethyl acetate = 4/1 – 7/3) to give diethyl 2-(1-ethoxyethylidene)malonate (5.02 g). To a solution of diethyl 2-(1-ethoxyethylidene)malonate (4.13 g) in ethanol (15 mL) were added formamidine hydrochloride (1.73 g) and a solution of potassium hydroxide (2.21 g) in water (7.5 mL), and the mixture was stirred at room temperature for 2 days. The reaction mixture was neutralized by adding acetic acid. To the mixture was added ethyl acetate (30 mL), and the mixture was stirred at room temperature for 30 minutes. The insoluble material was removed by filtration, and the filtrate was concentrated under reduced pressure. The residue was purified by column chromatography on silica gel (eluent: ethyl acetate – ethyl acetate/methanol = 9/1) to give the title compound (1.5 g).

The synthetic route of Diethyl 2-(1-ethoxyethylidene)malonate has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Kissei Pharmaceutical Co., Ltd.; EP2143724; (2010); A1;,
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Share a compound : Diethyl 2-(1-ethoxyethylidene)malonate

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. 3044-06-2, name is Diethyl 2-(1-ethoxyethylidene)malonate, This compound has unique chemical properties. The synthetic route is as follows., COA of Formula: C11H18O5

In a round-bottom flask, equipped with a stirrer, thermometer and reflux condenser, mix under nitrogen in the specified order: 1 g (0.0048 mol) of BCD-BTK-13-14 and 1.18 g (0.0051 mol) of diethyl-2-(1- ethoxyethylidene)malonate. Heat the mixture for 2 hours at 125-130 . Distill off the residual solvent using a rotary evaporator. Take the mixture to the next step without additional purification. Yield: 1.88 g (99%).

According to the analysis of related databases, 3044-06-2, the application of this compound in the production field has become more and more popular.

Reference:
Patent; JOINT STOCK COMPANY “BIOCAD”; GAVRILOV, Aleksey Sergeevich; ALESHUNIN, Pavel Aleksandrovich; GORBUNOVA, Svetlana Leonidovna; REKHARSKY, Mikhail Vladimirovich; KOZHEMYAKINA, Natalia Vladimirovna; KUKUSHKINA, Anna Aleksandrovna; KUSHAKOVA, Anna Sergeevna; MIKHAYLOV, Leonid Evgen`evich; MOLDAVSKY, Alexander; POPKOVA, Aleksandra Vladimirovna; SILONOV, Sergey Aleksandrovich; SMIRNOVA, Svetlana Sergeevna; IAKOVLEV, Pavel Andreevich; (197 pag.)WO2018/92047; (2018); A1;,
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Simple exploration of C11H18O5

Synthetic Route of 3044-06-2,Some common heterocyclic compound, 3044-06-2, name is Diethyl 2-(1-ethoxyethylidene)malonate, molecular formula is C11H18O5, 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 mixture of l-ethyl-lH-pyrazol-5-amine (16 gm, 0.144 moles) (example 2) and 2-(l-ethoxy-ethylidene)-malonic acid diethyl ester (29 gm, 0.12 moles) (example 3) was stirred at 1200C for about 2 hrs. When the reaction was complete on TLC, crude reaction mixture was concentrated in vacuo to remove ethanol, which was formed as byproduct. Crude residue was taken in phosphorous oxychloride (50 ml) and heated at 115 C for about 12-13 hrs. The reaction mixture was poured into ice-cooled water with continuous stirring. Solid which precipitated out was filtered and dried under vacuum to afford title compound as creamy white solid.Yield: 12 gm (57.17%) m/z: (M++l) 268.28

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route Diethyl 2-(1-ethoxyethylidene)malonate, its application will become more common.

Reference:
Patent; RANBAXY LABORATORIES LIMITED; RUDRA, Sonali; GUPTA, Nidhi; CHANDRAKANT, Kakade, Ganesh; JAIN, Tarun; VOLETI, Sreedhara, Rao; RAY, Abhijit; DASTIDAR, Sunanda G.; VIJAYKRISHNAN, Lalitha; WO2010/46791; (2010); A1;,
Ester – Wikipedia,
Ester – an overview | ScienceDirect Topics

New downstream synthetic route of Diethyl 2-(1-ethoxyethylidene)malonate

Electric Literature of 3044-06-2,Some common heterocyclic compound, 3044-06-2, name is Diethyl 2-(1-ethoxyethylidene)malonate, molecular formula is C11H18O5, 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.