Month: August 2021

Adding a certain compound to certain chemical reactions, such as: 16313-66-9, name is 2-Amino-5-bromobenzamide, belongs to amides-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 16313-66-9, Recommanded Product: 2-Amino-5-bromobenzamide

General procedure: A dry 50 mL flask was charged with 2-aminobenzamides 1 (2.1 mmol), 5,5-dimethyl-1,3-cyclohexanedione 2 (0.280 g, 2.0 mmol), iodine (0.026 g, 0.01 mmol) and toluene (10.0 mL). The mixture was stirred at 50 C until the reactant 1 was consumed. After the completion of the reaction monitored by TLC, toluene was recovered by distillation under reduced pressure, and the residue was purified by recrystallization in EtOH to give products 4.

If you are interested in these compounds, you can also browse my other articles.Thank you for taking the time to read this article. I hope you enjoyed it.

Reference:
Article; Lu, Lian; Zhang, Mei-Mei; Jiang, Hong; Wang, Xiang-Shan; Tetrahedron Letters; vol. 54; 8; (2013); p. 757 – 760;,
Amide – Wikipedia,
Amide – an overview | ScienceDirect Topics

Application of 60144-53-8, The chemical industry reduces the impact on the environment during synthesis 60144-53-8, name is tert-Butyl (4-fluorophenyl)carbamate, I believe this compound will play a more active role in future production and life.

Intermediate 1; 6-Fluorospiro[3,l-benzoxazine-4,4′-piperidin]-2(lH)-one; hydrochloride A mixture of 48.96 g (232 mmol) (4-fluoro-phenyl)-carbamic acid tert-butgamma ester and 300 mL tert-BuLi ( 1.7 M in hexane) in 380 mL THF at -70 0C was stirred for 50 min and afterwards 2.5 h at -200C. 44.3 g (223 mmol) 4-oxo-piperidine-l-carboxylic acid tert-butgamma ester (commercially available) in 180 mL THF was added at -70 0C and 60 mg KOtBu at 15 0C. The mixture was stirred at room temperature for 14 h. NH4Cl aq. was added, the organic phase was washed with saturated NaCl aq., and the aqueous phase was extracted with a mixture of THF and ethyl acetate. The combined organic phases were dried with Na2SC>4 and evaporated to dryness. The residue was titurated with diethyl ether, filtered off, washed with diethyl ether and dried to yield 31 g of tert-hutyi 6-fluoro- 2-oxo-l,2-dihydro-l ‘H-spiro[3,l -benzoxazine-4,4’-piperidine]-l ‘-carboxylate (MS (m/e): 335.5 (MH”) ) which was used without further purification in the consecutive step. 300 mL dioxane and 136 mL 4N HCl in dioxane was added and stirred at room temperature for 18 h. The precipitate was filtered off, washed with dioxane and diethyl ether and dried in vacuum. 21 g (36 %) of the title compound was yielded as light yellow solid. MS (m/e): 237.1 (MH+).

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, tert-Butyl (4-fluorophenyl)carbamate, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; F. HOFFMANN-LA ROCHE AG; WO2008/81012; (2008); A1;,
Amide – Wikipedia,
Amide – an overview | ScienceDirect Topics

Electric Literature of 2835-68-9, 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. 2835-68-9, name is 4-Aminobenzamide belongs to amides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

General procedure: To a mixture of 3-chloro-5-[(3-hydroxy-4-methylphenyl)amino]-4H-1,2,6-thiadiazin-4-one (7) (53.9 mg, 0.200 mmol), Pd[3,5-(F3C)2C6H3]3 (5.3 mg, 1.25 mol %), DPEPhos (5.3 mg, 5 mol %), powdered dry K2CO3 (66.4 mg, 0.480 mmol) and 3-aminobenzamide (30.0 mg, 0.220 mmol) was added dioxane (5 mL). The stirred suspension was then deaerated by bubbling of Ar through it for 5 min and then heated at reflux under Ar until complete consumption of the starting thiadiazine (TLC, 2 h). The mixture was cooled to ca. 20 C, then adsorbed onto silica and chromatographed (n-hexane/acetone, 50:50) to give the title compound 1 (63.1 mg, 85%) as orange needles, m.p. 297-298 C (from THF)

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

Reference:
Article; Asquith, Christopher R. M.; Godoi, Paulo H.; Cou ago, Rafael M.; Laitinen, Tuomo; Scott, John W.; Langendorf, Christopher G.; Oakhill, Jonathan S.; Drewry, David H.; Zuercher, William J.; Koutentis, Panayiotis A.; Willson, Timothy M.; Kalogirou, Andreas S.; Molecules; vol. 23; 5; (2018);,
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. 156731-40-7, name is 1-(Boc-amino)-3-butene, This compound has unique chemical properties. The synthetic route is as follows., COA of Formula: C9H17NO2

3-chloro-perbenzoic acid (3 equiv) is added to an ice-cooled solution of t-butyl but-3-enyl- carbamate (1 equiv) in CH2CI2 in an inert atmosphere and stirred at 40 for 3 hours. The mixture obtained is cooled to 5 and quenched with saturated aq. sodium bisulfite solution. After extraction with CH2CI2, the combined organic layers obtained are washed 3 times with saturated aq. potassium carbonate solution, dried, filtered and concentrated.(+/-)-t-butyl (2-oxiranyl-ethyl)-carbamate is obtained.

According to the analysis of related databases, 156731-40-7, the application of this compound in the production field has become more and more popular.

Reference:
Patent; NOVARTIS AG; NOVARTIS PHARMA GMBH; WO2007/48771; (2007); A1;,
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. 2675-89-0, name is 2-Chloro-N,N-dimethylacetamide, A new synthetic method of this compound is introduced below., HPLC of Formula: C4H8ClNO

Example 5.2Preparation of Cy-O-CH2-CONMe2 (Product 2-R1=Cy)Cyclohexanol (12.2 g, 0.11 mol) and toluene (42.2 g) are loaded In a 250 mL reactor. The temperature of this mixture is brought to 30 C. Soda (5.6 g, 0.14 mol) is then introduced with portions of about 2 g. The reaction mixture is mechanically stirred. After maintaining the stirring for ten minutes at 30 C., chlorodimethylacetamide (11.6 g, 0.09 mol) is added dropwise directly into the mass within 0.5 hour. The reaction medium is maintained with stirring at 30 C. for 5 hours. Distilled water is introduced until the totality of the salts are dissolved (about 30 mL). The organic phase is recovered and the solvents are distilled under partial pressure and the desired product is obtained, 12 g, with a yield of 72%.

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; Vidal, Thierry; Guglieri, Massimo; Jentzer, Olivier; US2012/302791; (2012); A1;,
Amide – Wikipedia,
Amide – an overview | ScienceDirect Topics

Adding a certain compound to certain chemical reactions, such as: 918538-04-2, name is Pyrrolo[2,1-f][1,2,4]triazine-2,4(1H,3H)-dione, belongs to amides-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 918538-04-2, SDS of cas: 918538-04-2

To a co-solvent of diisopropylethylamine (4.5 mL) and toluene (2OmL) was added intermediate 5? (1.6g, 10.4mmoL) and POC13 (2.94mL). The mixture was heated at 120C in a sealed tube for 20h, then poured into an ice-cooled saturated sodium bicarbonate solution (5OmL). Stirred for 1 5mm. Extracted with CH2C12 (3x5OmL). Combined organic layers were washed with brine (lx5OmL), dried (Mg504) and concentrated. Column chromatography purification (50-100% CH2C12 in hexanes) afforded the desired dichloride 1 as a light brown solid (1.2g, 86% yield). ?H NMR (CDC13): oe 6.98(1H, m), 7.05 (1H, m),7.86 (1H, m); MS: 187 (M+W).

At the same time, in my other blogs, there are other synthetic methods of this type of compound, Pyrrolo[2,1-f][1,2,4]triazine-2,4(1H,3H)-dione, and friends who are interested can also refer to it.

Reference:
Patent; SUZHOU KINTOR PHARMACEUTICALS, INC.; GUO, Chuangxin; TONG, Youzhi; (160 pag.)WO2017/219800; (2017); 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. 67442-07-3, name is 2-Chloro-N-methoxy-N-methylacetamide, This compound has unique chemical properties. The synthetic route is as follows., category: amides-buliding-blocks

To a stirred suspension of Intermediate B (3.00 g, 14.08 mmol) in THF (50 ml_) was added chlorotrimethylsilane (3.57 mL, 28.16 mmol). The mixture was stirred at rt for 3 h. The mixture was placed in a water ice bath and 2-propylmagnesium chloride (2M in THF; 29.6 mL, 59.14 mmol) was added dropwise. The suspension immediately went into solution. The ice bath was removed and the mixture was stirred at rt for 3 h. The mixture was placed in an ice bath and 2- chloro-AA-methoxy-AA-methylacetamide (2.91 g, 21.12 mmol) was added in one portion. The ice bath was once again removed and the reaction was stirred at rt for 16 h. The reaction was poured over a mixture of ice and saturated, aqueous ammonium chloride (250 mL). The mixture was allowed to warm to rt and EtOAc (200 mL) was added. The undissolved solid was collected by filtration to afford 636 mg (21percent) of the desired product. The layers of the filtrate were separated and and the aqueous phase was extracted with EtOAc (2 x 100 mL). The combined organic layers were washed with brine, dried (Na2SO4), and concentrated to dryness. The crude solid was triturated with EtOAc to provide an additional 1.62 g (55percent) of the desired product, for a combined yield of 2.26 g (76percent). ES-MS m/z 211.47 [M+H]+, HPLC RT (min) 1.67.

According to the analysis of related databases, 67442-07-3, the application of this compound in the production field has become more and more popular.

Reference:
Patent; BAYER PHARMACEUTICALS CORPORATION; WO2007/56170; (2007); A2;,
Amide – Wikipedia,
Amide – an overview | ScienceDirect Topics

Synthetic Route of 13621-50-6, The chemical industry reduces the impact on the environment during synthesis 13621-50-6, name is Ethyl 3-amino-3-thioxopropanoate, I believe this compound will play a more active role in future production and life.

Ethyl 2-amino-4-isopropyl-6-thio-5-cyano-1,4-dihydropyridine-3-carboxylate (IV). 1.0 g (10 mmol)of cyanothioacetamide II and a solution of sodiumethylate prepared from 0.23 g (10 mmol) of sodiumand 15 mL of anhydrous ethanol were added to a solution of 0.91 mL (10 mmol) of isobutyral Ia in15 mL of anhydrous ethanol at 20C. The reactionmixture was stirred during 5 min, then 1.5 g (10 mmol)of CH-acid III was added, and the mixture was stirredduring 30 min and incubated during 48 h. Next, themixture was diluted with 10% hydrochloric acid to pH5 upon stirring and incubated at room temperatureduring 48 h. The formed precipitate was filtered offand washed sequentially with water, ethanol, andhexane (Tables 1 and 2). Mass spectrum, m/z (Irel, %):266 (100) [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, Ethyl 3-amino-3-thioxopropanoate, other downstream synthetic routes, hurry up and to see.

Reference:
Article; Dyachenko; Karpov; Dyachenko; Russian Journal of General Chemistry; vol. 85; 5; (2015); p. 1063 – 1068; Russian Journal of General Chemistry; vol. 85; 5; (2015); p. 1063 – 1068,6;,
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. 1118-69-0, name is N-Isopropylacetamide, A new synthetic method of this compound is introduced below., SDS of cas: 1118-69-0

A 100 mL Schlenk flask fitted with a reflux condenser was charged with tetrakis(dimethylamido)zirconium (0.200 g, 0.748 mmol) and toluene (10 mL). A solution of N-isopropylacetamide (0.302 g, 2.99 mmol) in toluene (10 mL) was added slowly and the resultant mixture was refluxed for 3 h. Upon cooling to room temperature, the volatile components were removed under reduced pressure and sublimation of the crude solid at 110 C/0.05 Torr afforded 3 as colorless crystals (0.188 g, 51%): mp 206-209 C; IR (Nujol, cm-1) 1576 (s), 1456 (s), 1403 (s), 1363 (s), 1342 (s), 1319 (m), 1186 (s), 1170 (m), 1126 (m), 1051 (m), 987 (m), 886 (m), 822 (m), 814 (m), 614 (s), 582 (s); 1H NMR (C6D6, 23 C, delta) 3.34 (septet, J = 6.2 Hz, 4H, CH(CH3)2), 1.71 (s, 12H, CH3), 1.24 (d, J = 6.2 Hz, 24H, CH(CH3)2); 13C{1H} NMR (C6D6, 23 C, ppm) 183.00 (s, C=O), 48.94 (s, CH(CH3)2), 23.86 (s, CH(CH3)2), 17.06 (s, CH3). Anal. Calcd for C20H40N4O4Zr: C, 48.85; H, 8.20; N, 11.39. Found: C, 48.69; H, 8.06; N, 11.44.

The synthetic route of 1118-69-0 has been constantly updated, and we look forward to future research findings.

Reference:
Article; Karunarathne, Mahesh C.; Baumann, Joseph W.; Heeg, Mary Jane; Martin, Philip D.; Winter, Charles H.; Journal of Organometallic Chemistry; vol. 847; (2017); p. 204 – 212;,
Amide – Wikipedia,
Amide – 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. 513-74-6, name is Ammonium carbamodithioate belongs to amides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below. category: amides-buliding-blocks

Methyl Dithiocarbamate (I) [2] In a 500mL three-necked flask, provided with a gas-inlet tube, a stirrer, and a gas outlet combined with a thermometer, are placed dry THF(140mL) and carbon disulfide (16.7g, 0.22mol). Ammonia is then introduced with continuous stirring, the flow of ammonia being adjusted in such a way that a slow stream is leaving the flask. The temperature is allowed to rise to 40-45 °C and is kept at that level by occasional cooling. When, after 1h, no more heat is evolved and the temperature has dropped to 35 °C, the flask is evacuated (rotary evaporator) to remove some dissolved ammonia. Water (25mL) is then added to dissolved the white precipitate. To the resultant mixture of THF and aqueous ammonium dithiocarbamate, dimethylsulfate (25.2g, 0.2mol) is added with vigorous stirring. During the addition (which requires 30min), the temperature of the mixture is allowed to rise to 45-50 °C and is maintained at that level for 15 min by occasional cooling. Then, concentrated aqucous ammonia (5mL) is added to destroy excess dimethyl sulfate and stirring is continued for 15min. The upper layer is separated and dried with magnesium sulfate (without being washed). The aqueous layer is extracted with EA (3*20mL) and the organic phases are combined. The solution is concentrated in a water-pump vacuum and the last traces of solvent are removed at 0.5-1 torr by means of an oil pump to leave nearly pure methyl dithiocarbamate(I); yield: 20g (93percent, calculated on dimethyl sulfate).

The synthetic route of 513-74-6 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Shin Nippon Biomedical Laboratories, Ltd.; SUZUKI, Nobuyuki; YAMASHITA, Hidetoshi; (156 pag.)EP3018125; (2016); A1;,
Amide – Wikipedia,
Amide – an overview | ScienceDirect Topics