Category: 108-13-4

108-13-4, name is Malonamide, belongs to amides-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. name: Malonamide

B-1. 1,2-Dihydro-5-(4-methoxyphenyl)-2-oxonicotinamide–A mixture containing 82.1 g. of 3-dimethylamino-2-(4-methoxyphenyl)-2-propenal, 63.15 g. of malonamide (97%), 54.0 g. of sodium methoxide and 800 ml. of methanol was refluxed with stirring for about 17 hours and chilled. The reaction mixture was filtered and the filtrate concentrated in vacuo to a volume of about 500 ml., acidified with acetic acid and chilled. The resulting solid was collected, dried at 90 C. in a vacuum oven to yield 25.25 g. of 1,2-dihydro-5-(4-methoxyphenyl)-2-oxonicotinamide, m.p. 283-286 C.

The synthetic route of 108-13-4 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Sterling Drug Inc.; US4515797; (1985); A;,
Amide – Wikipedia,
Amide – 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. 108-13-4, name is Malonamide, A new synthetic method of this compound is introduced below., Formula: C3H6N2O2

[0533] Into a 3000-mL 3-necked round-bottom flask were placed a solution of sodium ethoxide (155 g, 2.28mol, 4.00 equiv) in ethanol (2000 mL), malonamide (233 g, 2.28mol, 4.00 equiv) and 5-chloro-l,3-dimethylpyrimidine-2,4(lH,3H)-dione (100 g, 571.43 mmol, 1.00 equiv). The resulting solution was heated to reflux for 20 min. Then it was cooled and concentrated under vacuum. The residue was diluted with 500 mL of H20, and then adjusted to pH 2 with HCl. The solid was collected by filtration and dried in an oven under reduced pressure. This resulted in 50 g (crude) of 5-chloro-2,6-dihydroxynicotinamide as a white solid.

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; ANACOR PHARMACEUTICALS, INC; JARNAGIN, Kurt; AKAMA, Tsutomu; WO2011/94450; (2011); A1;,
Amide – Wikipedia,
Amide – an overview | ScienceDirect Topics

Some common heterocyclic compound, 108-13-4, name is Malonamide, molecular formula is C3H6N2O2, 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 108-13-4

General procedure: An example of the preparation of the amide intermediate was carried out. Blocking the reaction vessel (when the amide intermediate is at a boiling point under normal pressure, etc.At or below the reaction temperature TB below) or to keep the reactor open (when the boiling point of the amide intermediate at normal pressure is higher than the reaction temperature TB described below), stirring is continued (600 r / min), The reaction temperature is changed to TB, and after maintaining the reaction temperature TB for TD hours, the reaction vessel is closed and connected to a vacuum pump, so that the degree of vacuum in the reaction vessel reaches 20-50 mbar (adjusted according to the type of nitrile product) to distill off As a nitrile product. The yield of the nitrile product was calculated and sampled for nuclear magnetic resonance spectroscopy and elemental analysis to characterize the obtained nitrile product. The specific reaction conditions and characterization results are shown in Tables A-6, A-7, A-8, A-9 and A-10 below. These characterization results indicate that the obtained nitrile product has an extremely high purity (99% or more).

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 108-13-4, its application will become more common.

Reference:
Patent; Sinopec Yangzi Petrochemical Co., Ltd.; Sinopec Corporation; Sun Hailong; Gao Yilong; Wei Yanyu; Chen Xinhua; Miao Jun; Li Na; Kan Lin; Bai Jiye; Chen Shaohui; Yang Aiwu; Xu Yuexing; (32 pag.)CN105016941; (2018); B;,
Amide – Wikipedia,
Amide – an overview | ScienceDirect Topics

Reference of 108-13-4,Some common heterocyclic compound, 108-13-4, name is Malonamide, molecular formula is C3H6N2O2, 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.

Step A:; To a solution of anyhydrous methanol (50 mL), sodium methoxide/methanol solution (61.47 mmol) and malonamide (4.50 g, 44.08 mmol) was added (E)-4-ethoxy-l,l,l-trifluoro-3-butene-2-one V-I (7.781 g, 46.28 mmol) and the mixture was heated to reflux for 2 hours. When the reaction was quenched by addition of water and the aqueous layer pH was adjusted to pH 1-3 with HCl. The mixture was concentrated to give compund V-2 (m/z (ES) (M+H)+= 207), which was used in the next step without further purification.

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

Reference:
Patent; MERCK & CO., INC.; WO2007/41052; (2007); A2;,
Amide – Wikipedia,
Amide – an overview | ScienceDirect Topics

Some common heterocyclic compound, 108-13-4, name is Malonamide, molecular formula is C3H6N2O2, 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. Recommanded Product: Malonamide

(1) Production of 1,2-dihydro-2-oxo-6-(trifluoromethyl)pyridine-3-carboxamide; Sodium methoxide (74g, 1.37 mol) was dissolved in methanol (1,000 mL), and malon diamide (100g, 0.979 mol) was added to this solution at room temperature. To this mixture, 4-ethoxy-1,1,1-trifluoro-3-buten-2-one (191g, 1.14 mol) was added dropwise at a temperature between 25 and 30C, and the resultant mixture was refluxed under heating for 2 hours. After cooling to 45C, concentrated hydrochloric acid was added to the mixed solution to give a pH of 3 to 4, and 500 mL of methanol was distilled off at normal pressure. To the residue, water (500 mL) was added, and the mixture was stirred for a day at room temperature. The resultant product was precipitated while cooling with ice. Thus obtained crystal was collected by filtration, washed with water, and then dried under reduced pressure, to obtain 167g of a subject compound (yield: 83%).

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 108-13-4, its application will become more common.

Reference:
Patent; KUMIAI CHEMICAL INDUSTRY CO., LTD.; IHARA CHEMICAL INDUSTRY CO., LTD.; EP1982978; (2008); A1;,
Amide – Wikipedia,
Amide – an overview | ScienceDirect Topics

108-13-4, name is Malonamide, belongs to amides-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. Formula: C3H6N2O2

To a solution of malonic-acid diamide (1 g) in DMF (15 mL), N,N dimethylformamide-dimethylacetal (1.4 g) added slowly. Then the mixture heated up to 50 C. and stirred for 3 h. The product isolated after concentration the mixture followed by crystallization (410 mg).1H NMR. (DMSO d6) delta: 7.45 and 7.02 (each bs, 4H, 2¡Á-NH2), 7.40 (s, 1H, -CH), 2.94 and 2.89 (2¡Ás, each 3H, 2¡Á-NCH3).13C NMR (DMSO d6) delta: 169.16 and 169.15 (2¡ÁCO), 151.08 (-HN-CH), 96.37 (C qvat.), 43.07 and 42.95 (2¡ÁNCH3).

The synthetic route of 108-13-4 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Dekany, Gyula; Agoston, Karoly; Bajza, Istvan; B¡ãjstrup, Marie; Kroeger, Lars; US2009/234111; (2009); A1;,
Amide – Wikipedia,
Amide – 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. 108-13-4, name is Malonamide, This compound has unique chemical properties. The synthetic route is as follows., HPLC of Formula: C3H6N2O2

EXAMPLE 3 4,6-Dihydroxy-2-trifluoromethylpyrimidine, Compound VI, starting material for Step 2 Sodium hydride (900 g, 57.5% dispersion in mineral oil; 518 g active NaH; 22.5M) was stirred with 7.5 L toluene in a 22 L round-bottomed flask. Butanol was added over 5 hr. so that the pot temperature was maintained at 40. The mixture was stirred an additional 16 hr. Malonamide (765 g; 7.5 M) was added, followed by ethyl trifluoroacetate (1065 g; 7.5 M). The ensuing reaction was exothermic; the mixture was then heated on a steam-bath for 3.5 hrs. It was then stirred at 23-25 for an additional 16 hrs. The mixture was extracted with water (1*4 L and 1*2 L). The combined aqueous extracts were treated with activated charcoal and filtered. The filtrate was maintained at 10-15 as it was acidified to pH 1-2 with 37% hydrochloric acid. The mixture was chilled to 5. The solid was isolated by filtration and dried at 50 in vacuo to give 600 g (44.4% yield) VI m.p. 255-256 (Lit. 265).

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 108-13-4.

Reference:
Patent; Bristol-Myers Squibb Co.; US4963678; (1990); A;,
Amide – Wikipedia,
Amide – an overview | ScienceDirect Topics