Category: 6629-04-5

Reference of 6629-04-5, 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. 6629-04-5 name is N-Cyanoacetylurethane, 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.

A 2 L, three-neck, round-bottom flask equipped with overhead stirring, a thermocouple, N2 inlet/outlet was charged with Int. 7 (75.0 g, 0.239 mol, 1 wt), acetic acid (600 mL, 8 vol), water (150 mL, 2 vol), and concentrated HC1 (71.3 mL, 0.95 vol). The resulting thin slurry was cooled to 6 C and a solution of NaN02 (16.8 g, 0.243 mol, 1.02 equiv) in water (37.5 mL, 0.5 vol) was added over a period of 10 min while maintaining a batch temperature below 10 C. After an additional 10 min of agitation between 5-10 C,HPLC analysis showed complete conversion of Int. 7 to the diazonium intermediate. A solution of NaOAc (54.5 g, 0.664 mol, 2.78 equiv) in water (225 mL, 3 vol) was added over a period of 6 min while maintaining a batch temperature below 10 C. N-cyanoacetylurethane (37.9 g, 0.243 mol, 1.02 equiv) was immediately added, the cooling was removed, and the batch naturally warmed to 8 C over 35 min. HPLC analysis showed complete consumption of the diazonium intermediate and the reaction was deemed complete. The batch warmed naturally to 21 C and was filtered through Sharkskin filter paper. The reactor and cake were washed sequentially with water (375 mL, 5 vol) twice. The collected orange solid was dried in a 35 C vacuum oven for 64 h to provide crude Int. 8 (104.8 g, 91%). A I L, three-neck, round-bottom flask equipped with overhead stirring, a thermocouple, and N2 inlet/outlet was charged with crude Int. 8 (104.4 g, 1 wt) and acetic acid (522 mL, 5 vol). The resulting slurry was heated to 50 C and held at that temperature for 1.5 h. The batch cooled naturally to 25 C over 2 h and was filtered through Sharkskin filter paper. The reactor and cake were washed sequentially with water (522 mL, 5 vol) and the cake conditioned under vacuum for 1.75 h. The light orange solid was dried to constant weight in a 40 C vacuum oven to provide 89.9 g (78% from Int. 7) of the desired product. 1H NMR (DMSO) was consistent with the assigned structure.

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

Electric Literature of 6629-04-5, 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. 6629-04-5 name is N-Cyanoacetylurethane, 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 solution of B (25 g, 160 mmol), propionaldehyde (9.3 g, 160 mmol) and Sg (5.1 g, 160 mmol) in DMF (30 mL) at 0C under nitrogen was added morpholine (7.9 g, 90 mmol). Reaction mixture was heated at 50C for 30 min, monitored by TLC. Solvent was removed in vacuo, and the mixture poured into ice water (50ml), extracted with EtOAc, washed with water and brine and concentrated. Crude material was purified by column chromatography (silica gel, EtOAc:PE = 1 : 1) to give 5 (6.8g, 18%) as a yellow solid.

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

Reference of 6629-04-5,Some common heterocyclic compound, 6629-04-5, name is N-Cyanoacetylurethane, molecular formula is C6H8N2O3, 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 solution of compound Al (3. 12g) and potassium carbonate (2.75g) in DMF (5OmL) is stirred at room temperature for 2 hours. 2.6mL carbon disulfide is added to the reaction suspension, and then kept stirring for 4 hours. After completion of the reaction, 100% ethanol is added to reaction mixture at 0C. Yellow precipitate is generated and filtered out. After washing with diethyl ether and drying under reduced pressure overnight, pale yellow solid, compound A2 is obtained in a yield of 92.3%. 1H-NMR (400MHz, DMSO-d6) 5 (ppm):14.92 (C3NHC4, s, 1H), 3.99 (C2H, q, J = 4.72Hz, 2H), 1.16 (C1H, t, J =4.72Hz, 3H). 13C- NMR (600MHz, DMSO-d6) 5 (ppm): 222.21 (C7), 164.35 (C4), 152.08 (C3), 125.16 (C6), 97.80 (C5), 59.09(C2), 14.50 (C1). HRMS (ESI) mlz calculated for C7H6N2O3S2K2+H308.9 172, found 308.9171. Formula is confirmed as C7H6N20352K2.

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

Reference:
Patent; RHODE ISLAND HOSPITAL; CHEN, Qian; YU, Hongchuan; CHEN, Yupeng; (123 pag.)WO2016/81522; (2016); A1;,
Nitrile – Wikipedia,
Nitriles – Chemistry LibreTexts

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. 6629-04-5, name is N-Cyanoacetylurethane belongs to nitriles-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below. Recommanded Product: N-Cyanoacetylurethane

Take aniline (compound c) 0.08mol, concentrated hydrochloric acid 45mL, 120mL water to make it dissolve,The solution was cooled to below 0C, and a 60 mL aqueous solution containing 0.11 mol of sodium nitrite was added dropwise.During the dropwise addition, the temperature was maintained below 0 C., and the mixture was stirred dropwise for 0.5 h. Ethyl 2-cyano-2-acetylcarbamate (compound d) dissolved in 400 mL of ethanol was added dropwise and 0.09 molA mixture of 0.27 mol sodium acetate was incubated for 3 h.The solid precipitated from the reaction mixture is filtered and the cake is washed with water.The pale yellow product was dried to give intermediate e(ethyl ((Z)-[2-cyano-2-(2-phenylhydrazono)acetyl]carbamate).

The synthetic route of 6629-04-5 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Liaoning University; Liu Ju; Chen Ye; Wang Yang; Li Jun; Zhou Ziyun; (22 pag.)CN107652300; (2018); A;,
Nitrile – Wikipedia,
Nitriles – Chemistry LibreTexts

Application of 6629-04-5, 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. 6629-04-5, name is N-Cyanoacetylurethane belongs to nitriles-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

Aniline (10.3 g, 0.11 mol) and hydrochloric acid (45 mL, 0.56 mol) were added to water (400 mL). The mixture was stirred and cooled down to 0 C. To the mixture was added dropwise an aqueous solution of NaNO2 (7.73 g, 0.11 mol) while controlling the temperature between 0 and 5 C. After the dropwise addition, the reaction was conducted at a temperature between 0 and 5 C. for 30 min. The obtained solution was reserved for future use. Intermediate a and sodium acetate (80 g, 0.98 mol) were added to ethanol (400 mL). The mixture was stirred and cooled down to 0 C. To the solution of Intermediate a was added dropwise the reserved solution while controlling the temperature between 0 and 5 C. After the dropwise addition, the reaction was conducted at a temperature between 0 and 5 C. for 2 h. The reaction is filtered by suction. The filtered cake was washed with water and dried to produce an orange solid (21.5 g) in a yield of 91.1%.

The synthetic route of N-Cyanoacetylurethane has been constantly updated, and we look forward to future research findings.

Reference:
Patent; XU, Hua; US2013/252958; (2013); A1;,
Nitrile – Wikipedia,
Nitriles – Chemistry LibreTexts

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. 6629-04-5, name is N-Cyanoacetylurethane, A new synthetic method of this compound is introduced below., Recommanded Product: 6629-04-5

EXAMPLE 1 A mixture of N-ethoxycarbonylcyanoacetamide (42 g), triethylorthoformate (40 g) and acetic anhydride (100 ml) is heated at reflux for one hour. The reaction is allowed to stand until cool and then is filtered, washing with ether, to yield alpha-cyano-beta-ethoxy-N-ethoxycarbonylacrylamide.

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; Zoecon Corporation; US4358591; (1982); A;; ; Patent; Zoecon Corporation; US4411839; (1983); A;; ; Patent; Imperial Chemical Industries Limited; Zoecon Corporation; US4307098; (1981); A;,
Nitrile – Wikipedia,
Nitriles – Chemistry LibreTexts

Adding a certain compound to certain chemical reactions, such as: 6629-04-5, name is N-Cyanoacetylurethane, belongs to nitriles-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 6629-04-5, Application In Synthesis of N-Cyanoacetylurethane

Take 15.0 of aniline, 90mL of concentrated hydrochloric acid, and 200mL of water to dissolve it.The solution is cooled below 0 C,A 70 mL aqueous solution containing 13.4 g of sodium nitrite was added dropwise,During the dropwise addition, keep the temperature below 0 C. After the dropwise addition is completed, keep warm and stir for 0.5h.Add 400 mL of ethanol to dissolve2-cyano-2-acetyl urethane 26.4gIt was incubated with a mixture of anhydrous sodium acetate 39.7 for 3 h.The solid precipitated in the reaction mixture was filtered, and the filter cake was washed with water.dryGot a pale yellow product,Intermediate[2-cyano-2- (2-phenylhydradino) acetyl] urethane(h).

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

Reference:
Patent; Liaoning University; Liu Ju; Chen Ye; Li Chunyan; Ding Shi; Gong Yilin; Shi Jiantao; Hao Xuechen; Wang Zhen; Yang Yaxing; (23 pag.)CN110684013; (2020); A;,
Nitrile – Wikipedia,
Nitriles – Chemistry LibreTexts

Related Products of 6629-04-5, A common heterocyclic compound, 6629-04-5, name is N-Cyanoacetylurethane, molecular formula is C6H8N2O3, 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: To the mixture of substituted anilines (0.08mol), concentrated hydrochloric acid (45.0mL) and water (120.0mL), aqueous solution of NaNO2 (60.0mL, 0.11mol) was added drop-wise under stir at a rate that the temperature below 0C, and the reaction mixture was stirred for 0.5h. A mixture of ethyl (2-cyanoacetyl)carbamate (13.7g, 0.09mol) and sodium acetate (24.0g, 0.27mol) in ethanol (400.0mL) was added drop-wise to the resulting diazonium salt solution below 0C and stirred for a further 2h. The precipitate was collected by filtration and washed with water (40.0 mL¡Á2), dried to give compounds 7a-f.

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:
Article; Zhao, Sijia; Zhang, Yu; Zhou, Hongyang; Xi, Shuancheng; Zou, Bin; Bao, Guanglong; Wang, Limei; Wang, Jiao; Zeng, Tianfang; Gong, Ping; Zhai, Xin; European Journal of Medicinal Chemistry; vol. 120; (2016); p. 37 – 50;,
Nitrile – Wikipedia,
Nitriles – Chemistry LibreTexts

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. 6629-04-5, name is N-Cyanoacetylurethane belongs to nitriles-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below. Recommanded Product: N-Cyanoacetylurethane

A mixture of 6-(4-amino-2,6-dichloro-phenylsuhcanyl)-4-isopropyl-2H-pyridazin-3-one (85) (3.40 g, 10.4 mmol) in water (135 mL) and concentrated hydrochloric acid (68 mL) cooled to 00C was treated with a solution of sodium nitrite (853 mg, 12.36 mmol) in water (7.0 mL) via Pasteur pipette under the surface of the reaction mixture. This was followed by a EPO water rinse (1.0 mL) of the Pasteur pipette. The resulting yellow mixture was stirred at 00C for 30 min. More concentrated hydrochloric acid (7.0 mL) was added. The reaction was stirred at 00C for an additional 1.3 h. The solids were removed by filtration through filter paper and were rinsed with water. The clear, yellow diazonium salt solution of the filtrate was quickly poured into a solution of cyanoacetylurethane (1.77 g, 11.33 mmol), pyridine (75 mL) and water (204 mL) cooled to 00C. Upon mixing, orange-red solids immediately formed. This mixture was stirred at 00C for 1 h. At this time, the solids were collected by filtration through filter paper. The solids were washed with water, air-dried under house vacuum for 2 h, and then dried under vacuum to afford (2-cyano-2-{ [3,5-dichloro-4-(5- isopropyl-6-oxo- 1 ,6-dihydro-pyridazin-3-ylsulfanyi)-phenyi] -hydrazono } -acetyl)-carbamic acid ethyl ester (86) (2.98 g, 58%) as an orange solid; ES(+)-HRMS m/e calcd for Ci9Hi8Cl2N6O4S (M+H)+ 497.0560, found 497.0559. Exact Mass = 496.0487; Molecular weight = 497.36

The synthetic route of 6629-04-5 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; F. HOFFMANN-LA ROCHE AG; WO2007/9913; (2007); A1;,
Nitrile – Wikipedia,
Nitriles – Chemistry LibreTexts