Category: 1462-12-0

Some common heterocyclic compound, 1462-12-0, name is Diethyl 2-ethylidenemalonate, molecular formula is C9H14O4, 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. Safety of Diethyl 2-ethylidenemalonate

General procedure: In the following three cases, Ia-1, Ia-2, and Ia-3 were used as free radical precursors, and reacted with Michael acceptor IIa to obtain addition product IIIa. The same reaction conditions were used: base K2HPO4, photocatalyst [Ir(ppy)2(dtbbpy)]PF6 (1 mol%),Solvent THF (concentration: 0.2 M), light source 8W blue LED strip, reaction temperature 40 C.

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 1462-12-0, its application will become more common.

Reference:
Patent; Sichuan University; Song Hao; Qin Yong; Xue Fei; Liu Xiaoyu; Zhang Dan; Wang Falu; Liu Jiazhen; Di Jiamei; Liao Qi; Lu Huifang; Zhu Min; He Liping; (29 pag.)CN108456156; (2018); A;,
Ester – Wikipedia,
Ester – an overview | ScienceDirect Topics

Reference of 1462-12-0, These common heterocyclic compound, 1462-12-0, name is Diethyl 2-ethylidenemalonate, 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 8 3,6-Dimethyl-5-oxoheptanoic acid 8-A. (1,4-Dimethyl-3-oxopentyl)propanedioic acid, diethyl ester A cold (0 C.) solution of 2,2,6,6-tetramethylpiperdine (10.241 gm, 72.5 mmol) in tetrahydrofuran (120 mL) was treated with n-butyl lithium (2.5 M in hexane, 29.0 mL, 72.5 mmol). The light yellow solution was stirred at 0 C. for 30. minutes, then cooled to -78 C. and treated with neat methyl isopropyl ketone (7.70 mL, 6.20 gm, 72 mmol) over a five-minute period. After 50 minutes, a solution of diethyl ethylidenemalonate (10.000 gm, 53.7 mmol) in tetrahydrofuran (7 mL) was added to the above mixture over a 10-minute period. After 50 minutes, the mixture was quenched with glacial acetic acid (5.0 ml) and warmed to room temperature. The mixture was poured into 50% saturated ammonium chloride and extracted with ethyl ether. The ethyl ether extract was washed with 1 N hydrochloric acid, water, and brine, then dried (magnesium sulfate), filtered and stripped to give a pale yellow oil. Distillation of the oil (P=0.15-0.2 mm Hg) afforded compound 8-A (10.883 gm, 74%) as a colorless liquid which boiled at 110-114 C. Thin layer chromatography: Rf =0.25 (20% ethyl acetate in hexane).

The synthetic route of 1462-12-0 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; E. R. Squibb & Sons, Inc.; US5072023; (1991); A;,
Ester – Wikipedia,
Ester – an overview | ScienceDirect Topics

Reference of 1462-12-0, 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. 1462-12-0, name is Diethyl 2-ethylidenemalonate belongs to esters-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

A solution of diethyl ethylidene malonate A (96 g; 0.51 mol), S-methyl isothiourea (71.1 g; 0.79 mol) and triethylamine (80 mL) in 530 mL of abs. ethanol, was refluxed for 3 h under magnetic stirring. The reaction mixture was filtered, and the ethanol concentrated under vacuum, water was added (400 mL) and extracted with ethyl acetate. The organic phase was dried over anhydrous sodium sulphate and concentrated. The crude reaction mixture was purified by silica gel column chromatography (eluant: n-hexane/ethyl acetate=7/3) to yield compound B (63.7 g; 55%) as a pure solid. 1H-NMR (400 Mhz, DMSO-d6), ppm: 1.16 (d, j=6.6 Hz, 3H); 1.17 (t, j=7.2 Hz, 3H); 3.29 (d, j=10.5 Hz, 1H); 3.84 (dq, j=6.6, 10.5 Hz, 1H); 4.21 (m, 2H);

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-ethylidenemalonate, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; Pharmacia Italia S.p.A.; US2004/9993; (2004); A1;,
Ester – Wikipedia,
Ester – an overview | ScienceDirect Topics

Adding a certain compound to certain chemical reactions, such as: 1462-12-0, name is Diethyl 2-ethylidenemalonate, 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 1462-12-0, Formula: C9H14O4

General procedure: In the following examples, if, Ig, Ih, and Ii are radical precursors, respectively, and reacted with Michael acceptor II to obtain an addition product III.Using the optimal reaction conditions:Base K2HPO4, photocatalyst [Ir(ppy)2(dtbbpy)]PF6 (1 mol%), solvent acetone (concentration: 0.2 M), light source 34W blue LED bulb, reaction temperature 40 C.

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-ethylidenemalonate, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; Sichuan University; Song Hao; Qin Yong; Xue Fei; Liu Xiaoyu; Zhang Dan; Wang Falu; Liu Jiazhen; Di Jiamei; Liao Qi; Lu Huifang; Zhu Min; He Liping; (29 pag.)CN108456156; (2018); A;,
Ester – Wikipedia,
Ester – an overview | ScienceDirect Topics

Related Products of 1462-12-0, A common heterocyclic compound, 1462-12-0, name is Diethyl 2-ethylidenemalonate, molecular formula is C9H14O4, 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.

General procedure: Isatin Schiff base 2 (22.2 mg, 0.1 mmol), the corresponding electrophile (0.2 mmol), and catalyst I (6.0 mg, 0.01 mmol) were stirred in toluene or 1,2-DCE (0.3 mL) at the reported temperature for the appropriate time (Tables 2 and 3). In the case of the reactions carried out at 2 or -25 C, the reaction vessel containing the reagents and the solvent were cooled prior to mixing together. The reactions were followed by TLC (CH2Cl2-EtOAc, 20:1). The hydrolysis was carried out in situ by adding a mixture of THF and 10% aq HCl (3:1, 1 mL) with vigorous stirring for 15-20 min. The reaction mixture was transferred to separatory funnel, diluted with H2O (10 mL), and extracted with CH2Cl2 (3 × 10 mL). The combined extracts were dried (MgSO4), concentrated, and the product was isolated by column chromatography. The racemic standards were obtained by the same procedure using 1 equiv of K2CO3 as catalyst. After the completion of the reaction, the mixture was separated from K2CO3, hydrolyzed, and purified in the same manner.

The synthetic route of 1462-12-0 has been constantly updated, and we look forward to future research findings.

Reference:
Article; ?ari, Sergei; Metsala, Andrus; Kudrjashova, Marina; Kaabel, Sandra; Jaerving, Ivar; Kanger, Tonis; Synthesis; vol. 47; 6; (2015); p. 875 – 886;,
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. 1462-12-0, name is Diethyl 2-ethylidenemalonate belongs to esters-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below. Computed Properties of C9H14O4

Synthesis of compound 9.4. To a solution of compound 9.3 (1.3g, 4.86mmol, 1.0 equiv) and diethyl 2-ethylidenemalonate (0.9 g, 4.86mmol, 1.0 equiv) in ethanol (13 mL) was added sodium ethoxide (0.59g, 8.74mmol, 1.8 equiv) at room temperature. The mixture was refluxed for 3 hours then the solvent was removed under reduced pressure. The crude material was purified via flash column chromatography to yield compound 9.4 (2.6g, 65%>). MS (ES): m/z 409 [M+H]+.

The synthetic route of 1462-12-0 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; NIMBUS LAKSHMI, INC.; MASSE, Craig E.; GREENWOOD, Jeremy Robert; ROMERO, Donna L.; HARRIMAN, Geraldine C.; WESTER, Ronald T.; SHELLEY, Mee; KENNEDY-SMITH, Joshua Jahmil; DAHLGREN, Markus; WO2015/131080; (2015); A1;,
Ester – Wikipedia,
Ester – an overview | ScienceDirect Topics

Some common heterocyclic compound, 1462-12-0, name is Diethyl 2-ethylidenemalonate, molecular formula is C9H14O4, 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. Product Details of 1462-12-0

General procedure: To a mixture of alkene 1 (0.5 mmol), aldehyde 2 (2.5 mmol), and FeCl2 (1.6 mg, 0.0125 mmol), acetonitrile (3.0 mL) was added under nitrogen at room temperature. Then tert-butyl hydroperoxide 3 (TBHP, 2.0 mmol, 5-6 M in decane) was dropped into the mixture under nitrogen at room temperature. The resulting mixture was stirred under 85 oC for 1 h. The temperature of reaction was cooled to room temperature. The resulting reaction solution was directly filtered through a pad of silica by ethyl acetate. The solvent was evaporated in vacuo to give the crude products. NMR yields are determined by 1H NMR using dibromomethane as an internal standard. Solvent was evaporated and the residue was purified by flash column chromatography on silica gel with ethyl acetate/petroleum ether as eluent to afford the pure product 4.

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 1462-12-0, its application will become more common.

Reference:
Article; Liu, Kaisheng; Li, Yuanming; Zheng, Xiaojian; Liu, Weiping; Li, Zhiping; Tetrahedron; vol. 68; 50; (2012); p. 10333 – 10337;,
Ester – Wikipedia,
Ester – an overview | ScienceDirect Topics