Month: July 2021

Application of 2895-21-8, 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. 2895-21-8, name is N-Isopropyl-2-chloroacetamide, This compound has unique chemical properties. The synthetic route is as follows.

A solution of 4-{[6-(3-chlorophenyl)-4-oxo-4,5-dihydropyrazolo[1 ,5-a]pyrazin-2-yl]oxy}butyl acetate (0.25 g, P23) and potassium carbonate (0.18 g) in dry acetonitrile (6 ml.) 2-chloro- N-(1-methylethyl)acetamide (0.1 g) was added and the reaction was stirred at 8O0C on. After cooling the mixture was diluted with AcOEt and washed with chilly water and brine. The organic phase was dried, filtered and the solvent evaporated under vacuum. The crude was dissolved in THF (20 ml_), lithium hydroxyde (5 ml_, 0.5 M solution in water) was added and the mixture was stirred at RT for 2h. Solvent was removed under reduced pressure; the residue was taken up with AcOEt and washed with water. The organic phase was dried, filtered and evaporated under vacuum to give a mixture of the title compounds (0.21 g) that was used in next step without further purification.MS ( m/z): 433 [MH]+.

The chemical industry reduces the impact on the environment during synthesis N-Isopropyl-2-chloroacetamide. I believe this compound will play a more active role in future production and life.

Reference:
Patent; GLAXO GROUP LIMITED; WO2009/130232; (2009); A1;,
Amide – Wikipedia,
Amide – an overview | ScienceDirect Topics

Related Products of 53844-02-3,Some common heterocyclic compound, 53844-02-3, name is Benzyl (2-bromoethyl)carbamate, molecular formula is C10H12BrNO2, 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.

Treat a -78 C solution of diisopropylamine (35 g, 0.346 mol) in THF (300 mL), under N2, drop-wise with a solution of n-butyllithium (2.5 M, 127 mL, 0.317 mol), warm to -30 C for 0.5 h, re-cool to -78C and treat drop-wise with a solution of isobutyronitrile (19.9 g, 0.288 mol) in THF (100 mL). Stir the mixture at -78C for 0.5 h, treat with a solution of benzyl (2-bromoethyl)carbamate (74 g, 0.288 mol) in THF (100 mL), stir at – 78C for 1 h, then warm to RT and stir overnight. Treat the mixture with H20, separate the layers, extract the aqueous layer with EtOAc, wash the combined organics with brine, dry over Na2S04, concentrate to dryness and purify via silica gel chromatography (EtOAc/Petroleum ether) to afford the title compound (15 g, 21 % yield). MS (m/z): 247.2 (M+l).

The synthetic route of 53844-02-3 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; DECIPHERA PHARMACEUTICALS, LLC; ELI LILLY AND COMPANY; FLYNN, Daniel L.; KAUFMAN, Michael D.; VOGETI, Lakshminarayana; WISE, Scott C.; LU, Wei-Ping; SMITH, Bryan D.; CALDWELL, Timothy M.; PATT, William C.; HENRY, James Robert; HIPSKIND, Philip Arthur; PENG, Sheng-Bin; WO2013/134298; (2013); A1;,
Amide – Wikipedia,
Amide – an overview | ScienceDirect Topics

Related Products of 6973-09-7, A common heterocyclic compound, 6973-09-7, name is 5-Amino-2-methylbenzenesulfonamide, molecular formula is C7H10N2O2S, 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.

To a stirred suspension of the product of Intermediate Example 4 (1.1 g, 3.7 mmol) in 10 mL of THF, was added 5-amino-2-methylbenzenesulfonamide (0.70 g, 3.8 mmol, 1.0 equiv) at room temperature. The reaction mixture was heated at reflux for 3 h, then 4 M HCI in 1 ,4-dioxane (18 muL, 0.072 mmol) was added in one portion. After 5 h, the suspension was cooled to room temperature, and filtered. The resulting solid was washed with 16 mL of THF and dried in the air to yield 1.6 g (92%) of 5-({4- [(2,3-dimethyl-2H-indazol-6-yl)methylamino]-2-pyrimidinyl}amino)-2-methylbenzene sulfonamide monohydrochloride as a light yellow solid.

The synthetic route of 6973-09-7 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; SMITHKLINE BEECHAM CORPORATION; WO2007/64753; (2007); A2;,
Amide – Wikipedia,
Amide – an overview | ScienceDirect Topics

Adding a certain compound to certain chemical reactions, such as: 6274-22-2, name is 4-Amino-N-methylbenzamide, 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 6274-22-2, name: 4-Amino-N-methylbenzamide

Thiophosgene (1.13 ml, 1.1 eq) is added dropwise to a solution cooled down to 0 C., of 4-amino-N-methylbenzamide (2 g, 1 eq) and triethylamine (5.6 ml, 3 eq) in tetrahydofuran (260 ml). The mixture is stirred for 30 minutes at 0 C. then the cold bath is removed and stirring is continued for another 30 minutes. Water (100 ml) and diethyl ether (250 ml) are added to the mixture. After decantation and extractions, the organic phases are combined, washed with salt water, dried over Na2SO4 then concentrated under reduced pressure at 40 C. The solid obtained is recrystallized from a dichloromethane/petroleum ether mixture (2.2 g; 86% yield). NMR (1H, 400 MHz, DMSO-d6): delta 2.77 (d, 3H), 7.51 (AB, 2H), 7.88 (AB, 2H), 8.52 (m, 1H).

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, 4-Amino-N-methylbenzamide, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; Poitout, Lydie; Brault, Valerie; Sackur, Carole; Roubert, Pierre; Plas, Pascale; US2006/173036; (2006); A1;,
Amide – Wikipedia,
Amide – an overview | ScienceDirect Topics

Related Products of 4943-86-6, These common heterocyclic compound, 4943-86-6, name is 2-Amino-N-(4-chlorophenyl)benzamide, 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: A solution of the substituted benzamide (1equiv) and ortho-bromobenzaldehyde(1.41 mmol, 1 equiv) in acetonitrile (5mL) was treated with cyanuric chloride(0.022 mmol, 10 mole %). The reaction mixture was stirred at room temperature for 5-10 min and formed precipitate was filtered and recrystallised with ethanol to obtain the compounds 1, 6a, 6b and 16.

Statistics shows that 2-Amino-N-(4-chlorophenyl)benzamide is playing an increasingly important role. we look forward to future research findings about 4943-86-6.

Reference:
Article; Sharma, Moni; Mahar, Rohit; Shukla, Sanjeev K.; Kant, Ruchir; Chauhan, Prem M.S.; Tetrahedron Letters; vol. 54; 46; (2013); p. 6171 – 6177;,
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. 162787-61-3, name is 2-(Methylsulfonamido)benzoic acid, A new synthetic method of this compound is introduced below., Safety of 2-(Methylsulfonamido)benzoic acid

In a separate reaction vessel, O-Benzoic acid methanesulfamide(0.039g, 0.183 mmol),HATU(0.1 16g, 0.305 mmol), and pyridine(29ul, 0.366 mmol), were dissolved in anhydrous DMF (5 ml). The reaction mixture was stirred under nitrogen for 2 hours to activate the acid. When activation was approximately 80% complete by LC/MS (2 hr) the piperidine solution in DMF (0.028g, 0.121 mmol), along with DIPEA (86ul, 0.488mmol) were added. The reaction was stirred overnight while monitoring by LC/MS. Solvents were removed by rotary evaporation. The residue was taken up in DCM (100 ml)and washed with water (5 x 100 ml). The organic layer was collected, dried over MgS04, filtered and evaporated. The residue was taken up in DCM and columned on silica gel using a gradient of 0 to 10% MeOH to provide compound 18 : DCM. (Yield- 32.45 mg, 0.076 mmol, 62 %).1H-NMR (CD3CN, 300 MuEtazeta):delta 1.50 (m, 2H), 1.74 (m, 1H), 2.20 (bs, 1H), 2.31 (s, 3H), 2.43 (s, 1H), 2.99 (s, 3H), 3.10 (m, 1H), 3.35 (m, 1H), 6.22-6.46 (m, 1H), 7.25-7.70 (m, 4H), 8.80- 9.00 (m, 1H).

The synthetic route of 162787-61-3 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; GILEAD SCIENCES, INC.; BABAOGLU, Kerim; BOOJAMRA, Constantine, G.; EISENBERG, Eugene, J.; HUI, Hon Chung; MACKMAN, Richard, L.; PARRISH, Jay, P.; SANGI, Michael; SAUNDERS, Oliver, L.; SIEGEL, Dustin; SPERANDIO, David; YANG, Hai; WO2011/163518; (2011); A1;,
Amide – Wikipedia,
Amide – an overview | ScienceDirect Topics

Adding a certain compound to certain chemical reactions, such as: 98-64-6, name is 4-Chlorobenzenesulfonamide, 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 98-64-6, HPLC of Formula: C6H6ClNO2S

General procedure: To a round-bottom flask (500 mL) that contained a solution of aryl sulfonamide (6 mmol), 4-dimethyaminopyridine (DMAP, 13 mmol), and 1-[3-(dimethyamino)-propyl]-3-ethylcarbodiimide hydrochloride (EDCI, 13 mmol) in CH2Cl2 (150 mL) was added the synthesized cinnamic acid (6 mmol) at room temperature. The resulting mixture was stirred at room temperature for 12 h, then cooled to 5 °C, and acidified to pH 1 with addition of HCl aqueous solution (10percent), which was followed by extraction with CH2Cl2/MeOH (9:1, 3 .x. 100 mL). The combined organic layers were washed with H2O and brine, dried over Na2SO4, and concentrated in vacuo. The residue was subjected to silica gel chromatography or crystallization if necessary to afford the compounds (9a-16e) (Scheme 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, 4-Chlorobenzenesulfonamide, other downstream synthetic routes, hurry up and to see.

Reference:
Article; Luo, Yin; Qiu, Ke-Ming; Lu, Xiang; Liu, Kai; Fu, Jie; Zhu, Hai-Liang; Bioorganic and Medicinal Chemistry; vol. 19; 16; (2011); p. 4730 – 4738;,
Amide – Wikipedia,
Amide – an overview | ScienceDirect Topics

Application of 122334-37-6, 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. 122334-37-6, name is 4-Chloro-N-methoxy-N-methylbenzamide belongs to amides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

A -78 0C solution of 3-iodo-l -(6-methyl-pyridin-2-ylmethyl)-l H-quinolin-4-one (113 mg, 0.3 mmol, 1 equiv) in 3 mL of THF was treated with 1.65 mL of isopropyl magnesium chloride (1.1 equiv) for 2 hours. Then 4-chloro-N-methoxy-N-methyl- benzamide (46 muL, 1.2 equiv) was added and stirring continued at rt for 2 hours. The reaction was quenched by slow addition of saturated aqueous solution OfNH4Cl. Standard workup followed by HPLC purification gave 3-(4-chloro-benzoyl)-l-(6-methyl-pyridin-2-ylmethyl)- 1 H-quinolin-4-one. LCMS (ES) M+H 389.1

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, 4-Chloro-N-methoxy-N-methylbenzamide, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; CHEMOCENTRYX, INC.; WO2007/59108; (2007); A2;,
Amide – Wikipedia,
Amide – an overview | ScienceDirect Topics

Electric Literature of 6919-61-5, A common heterocyclic compound, 6919-61-5, name is N-Methoxy-N-methylbenzamide, molecular formula is C9H11NO2, 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.

To a solution of 5.0g (25.4 mmol) of tetaut-butyldimethyl-pent-4-ynylochiy-silane (prepared by the method of Koseki, Y.; Sato, H.; Watanabe, Y.; Nagasaka, T. Org. Lett. 2002, 4, 885-888) in 10OmL of THF at -78C under an atmosphere of N2 was added dropwise 10.2 mL (25.4 mmol) of 2.5 M nBuLi in hexane. After stirring for Ih at that temperature, 4.0 g (24.2 mmol) of N-methoxy-N-methyl benzamide (2-1) in 20 mL of THF was added, the cooling bath was removed, and stirring was continued for 3h at room temperature. The reaction was quenched with saturated aqueous NH4Cl, extracted with 2 x EtOAc, washed with brine, dried over Na2SO4, and concentrated. The crude material was loaded onto a 4Og silica gel cartridge and eluted with a gradient of 0 to 55% EtOAc in hexanes over 25 minutes to provide 6.3g (20.9 mmol, 87%) of the propargylic ketone (2-2) as a pale yellow oil. To a suspension of 2.2g (10.7 mmol) of CuBrOMS in 30 mL of THF at -78C was added 10.7 mL (21.4 mmol) of a 2.0 M solution of PhLi in dibutylether. After stirring for 1.5h, 2.7g (8.9 mmol) of the above prepared ketone 2-2 in 5mL of THF was added, and the mixture was allowed to stir for an additional 3h at -78C, and warmed to 00C for 15 minutes before being quenched with saturated aqueous NH4Cl. The mixture was partitioned with EtOAc, the layers were separated, the aqueous was extracted with 2 x EtOAc, the organics were combined, washed with brine, dried over Na2SO4, and concentrated. The crude material was loaded onto a 4Og silica gel cartridge and eluted with a gradient of 0 to 25% EtOAc in hexanes to provide 2.89g (7.6 mmol, 85%) of 2-3 as a yellow oil; NMR analysis indicated that there was a 1.1:1 mixture of E:Z isomers. Careful separation of a fraction of this material provided the pure isomers, whose identities were determined by ID NOE analysis. Data for 2-3-(E) (first to elute): 1HNMR (500 MHz, CDCl3) delta 8.0 (m, 2H), 7.6 – 7.4 (m, 8H), 7.1 (s, IH), 3.7 (t, J = 6.3 Hz, 2H), 3.1 (m, 2H), 1.75 (m, 2H), 0.9 (s, 9H), 0.01 (s, 6H) ppm. Data for 2-3-(Z) (second to elute): 1HNMR (500 MHz, CDCl3) delta 7.8 (m, 2H) 7.45 (m, IH), 7.35 (m, 2H), 7.25 – 7.1 (m, 5H), 6.7 (s, IH), 3.65 (t, J = 6.3 Hz, 2H), 2.65 (t, J = 7.6 Hz, 2H), 1.7 (m, 2H), 0.9 (s, 9H), 0.05 (s, 6H) ppm. Data for mixture 2-3: HRMS (ES) calc’d M + H for C24H32O2Si: 381.2245. Found: 381.2251

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; MERCK & CO., INC.; WO2006/7501; (2006); A2;,
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. 194920-62-2, name is tert-Butyl (3-(2-(2-(3-aminopropoxy)ethoxy)ethoxy)propyl)carbamate, A new synthetic method of this compound is introduced below., Quality Control of tert-Butyl (3-(2-(2-(3-aminopropoxy)ethoxy)ethoxy)propyl)carbamate

In four flasks (20mL), compound IX (0.45mmol in each) was dissolved in DMF (5mL in each) and afterwards, compounds I, II, V, or VI (2mmol), HOAt (3mmol), PyAOP (2mmol) and DIPEA (8mmol), were added to each flask. The reaction mixture of each flask was heated at 100C for 12h, diluted with water and extracted three times with DCM. Each organic layer was dried with anhydrous Na2SO4 and the solvent was removed under reduced pressure. Finally, each residue was purified by column chromatography using hexane/ethyl acetate as the solvent and thus compounds 5 (94%), 6 (91%), 7 (86%), or 8 (90%) were yielded, respectively.

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; Medina-O’Donnell, Marta; Rivas, Francisco; Reyes-Zurita, Fernando J.; Martinez, Antonio; Martin-Fonseca, Samuel; Garcia-Granados, Andres; Ferrer-Martin, Rosa M.; Lupianez, Jose A.; Parra, Andres; European Journal of Medicinal Chemistry; vol. 118; (2016); p. 64 – 78;,
Amide – Wikipedia,
Amide – an overview | ScienceDirect Topics