Month: July 2021

Electric Literature of 112434-18-1, 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. 112434-18-1, name is Benzyl (2,4-difluorophenyl)carbamate, This compound has unique chemical properties. The synthetic route is as follows.

Step 2-Preparation of (2,4-difluoro-3-formyl-phenyl)-carbamic acid benzyl ester (53)Into a round bottom flask was added (2,4-difluoro-phenyl)-carbamic acid benzyl ester (52, 3.83 g, 14.5 mmol) in tetrahydrofuran (148 ml, 1.82 mol). The solution was chilled to 78 C. and n-butyllithium (1.60 M in hexane, 19.1 mL, 30.0 mmol) was added over 30 minutes followed by the addition of, N,N-dimethylformamide (1.12 mL, 14.5 mol). The reaction mixture was allowed to warm to ambient temperature and was stirred overnight. The reaction mixture was poured into water and extracted with ethyl acetate. The organic layer was washed with brine, dried over sodium sulfate, concentrated and crystallized from ether to give compound 53 (3.0 g, 71%).

The chemical industry reduces the impact on the environment during synthesis Benzyl (2,4-difluorophenyl)carbamate. I believe this compound will play a more active role in future production and life.

Reference:
Patent; Spevak, Wayne; Cho, Hanna; Ibrahim, Prabha N.; Shi, Shenghua; Mamo, Shumeye; Gillette, Samuel J.; Zhu, Hongyao; US2008/167338; (2008); A1;,
Amide – Wikipedia,
Amide – an overview | ScienceDirect Topics

142-26-7, name is N-Acetylethanolamine, 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. category: amides-buliding-blocks

Example 5 This example illustrates an alternative method for producing (-)-halofenate. A 500-mL round-bottom flask with a magnetic stirrer is charged with 35.5 g (65.4 mmol) of the (-)-CPTA/(S)-(-)-1-(2-naphthyl)-ethylamine diastereomeric salt (98% ee), 89.0 g of 1,2-dichloroethane, and 35.5 mL of water. To the slurry is added 6.7 g (68 mmol) of 37% hydrochloric acid, and the mixture was stirred at ambient temperature to give two clear phases. The lower organic phase is removed and washed with 7.0 g of water. The organic phase is evaporated, then dissolved in 55.6 g of 1,2-dichloroethane and placed in a 250-mL round-bottom flask in a heating mantel with a magnetic stirrer and fitted with a reflux/distillation head. To the solution is added 7.5 mL (100 mmol) of thionyl chloride, and the solution is heated to reflux for 2 hours. Heating is continued to collect distillate. The solution is cooled to ambient temperature, then chilled in an ice bath for the addition of 25.85 g (251 mmol) of distilled N-acetylethanolamine (KF analysis 1176 and 1288 ppm water). The solution is added slowly with stirring to 9.90 g (71.6 mmol) of potassium carbonate in 36 g of water chilled in an ice bath. The reaction mixture is rinsed with 5 mL of 1,2-dichloroethane. The lower organic phase is removed and washed with 37 mL of water. The solution is evaporated to give an residue. The residue is treated with 54 g of heptane, and the solvent is removed to give a residue. To the residue is added 76 g of heptane, and the solvent is removed to give a residue. The residue is dissolved in 28 mL of 2-propanol at 40 C., then diluted with an additional 28 mL of 2-propanol and 334 mL of heptane. Cooling to ambient temperature gives a slurry which thickens upon cooling in an ice bath. After stirring for 2 hours, the solid is isolated by vacuum filtration, rinsed with 29 g of heptane, and dried to give (-)-halofenate.

The synthetic route of 142-26-7 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Metabolex, Inc.; US2007/73082; (2007); A1;,
Amide – Wikipedia,
Amide – an overview | ScienceDirect Topics

Synthetic Route of 67442-07-3, In the chemical reaction process, reaction time, type of solvent, can easily affect the result of the reaction, thereby determining the yield and properties of the reaction product. An updated downstream synthesis route of 67442-07-3 as follows.

[0541] A mixture of N-(4-chlorobenzyl)-2-(hydroxymethyl)-7-oxo-4,7-dihydrothieno[3,2-b]pyridine-6-carboxamide (100 mg, 0.288 mmol), potassium carbonate (60 mg, 0.43 mmol) and 2-chloro-N-methoxy-N-methylacetamide (200 mg) in DMF (1.5 mL) was shaken at room temp. for 48 hrs. The mixture was diluted with water (5 mL), and the resulting solid was collected by filtration. The crude solid was recrystallized from aq. ethanol to afford title compound (90 mg). The title compound is also a compound of formula I. [0542] Physical characteristics are as follows: [0543] 1H NMR (400 MHz, DMSO-d6) delta) 10.45 (1H), 8.73 (1H), 7.37 (4H); 7.26 (1H), 5.91 (1H), 5.47 (2H), 4.74 (2H), 4.54 (2H), 3.86 (3H), 3.16 (3H); HPLC ret time=2.86 min; MS (ES+) m/z 450, 452.

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; Larsen, Scott D.; May, Paul; Romines, Karen; Schnute, Mark E.; Tanis, Steven P.; US2004/138449; (2004); A1;,
Amide – Wikipedia,
Amide – an overview | ScienceDirect Topics

These common heterocyclic compound, 316146-27-7, name is N-(4-Bromophenyl)-3-phenylpropanamide, 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. SDS of cas: 316146-27-7

General procedures:; Scheme 2; An acid (1 equiv), HATU (1 equiv) and DIEA (3 equiv) were added to a solution of 4-bromo-aniline (1 equiv) in DMF. The mixture was stirred at room temperature until the starting material disappeared (detection by LC-MS). The solution was diluted with EtOAc and washed with saturated aqueous NaHCO3. The organic layer was dried over anhydrous sodium sulfate and concentrated in vacuo to give the crude bromide 2-1. The bromide 2-1 (1 equiv) and the boronic acid ester (1.5 equiv) were dissolved in degassed dioxane/H2O (5:1 by volume) in a sealed tube. Pd(PPh3)4 (0.03 equiv) and 2M solution Of K2CO3 (3 equiv) were added sequentially. The mixture was heated at 95 0C for 2h. After cooling to room temperature, the mixture was diluted with water and extracted with ethyl acetate. The organic layers were combined, dried over sodium sulfate and concentrated in vacuo. The residue was then purified by preparative HPLC to give the product 2-2 as a solid (65percent-80percent yield in two steps).; Example 27. N-(4-(lH-pyrazol-4-yl)phenv0-3-phenylpropanamide; Procedures in Scheme 2 were utilized to synthesize this compound. LC/MS: Ci8HnN3O (M+l) 292. Single peak at both 215 nm and 254 nm in analytical HPLC traces.

The synthetic route of N-(4-Bromophenyl)-3-phenylpropanamide has been constantly updated, and we look forward to future research findings.

Reference:
Patent; FENG, Yangbo; LOGRASSO, Philip; SCHROETER, Thomas; YIN, Yan; WO2010/36316; (2010); A1;,
Amide – Wikipedia,
Amide – an overview | ScienceDirect Topics

Some common heterocyclic compound, 194920-62-2, name is tert-Butyl (3-(2-(2-(3-aminopropoxy)ethoxy)ethoxy)propyl)carbamate, molecular formula is C15H32N2O5, 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: 194920-62-2

To a 25 mL round bottomed flask equipped with a magnetic stir bar, rubber septum, and argon inlet containing tert-butyl 3-(2-(2-(3-aminopropoxy)ethoxy)ethoxy)propylcarbamate (amine, 160 mg, 0.5 mmol), 2-azidoacetic acid (56 mg, 0.55 mmol, in 50% DCM solution), NaHCO3 (168 mg, 2 mmol), and 1 mL DMF was added EDC (115 mg, 0.6 mmol). The mixture was stirred at rt for 3 h and concentrated in vacuo. The crude product was purified by silica chromatography (gradient 5% to 90% EtOAc in hexane) to afford compound 141 as a clear oil (130 mg, 65%). MS(ESI) m/z 426 (M+Na+).

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 194920-62-2, its application will become more common.

Reference:
Patent; SIEMENS MEDICAL SOLUTIONS USA, INC.; WO2008/124703; (2008); A2;,
Amide – Wikipedia,
Amide – an overview | ScienceDirect Topics

Related Products of 6292-59-7, In the chemical reaction process, reaction time, type of solvent, can easily affect the result of the reaction, thereby determining the yield and properties of the reaction product. An updated downstream synthesis route of 6292-59-7 as follows.

c) A solution of 0.353 g of 4,6-dichloro-5-(2-methoxyphenoxy)-2-(thiophen-2-yl)-pyrimidine in 5 ml of DMSO was heated to 150° C. with 0.376 g of p-tert-butylbenzenesulphonamide for 30 minutes. The solution was concentrated in a high vacuum and the oily residue was poured on to ice, made acid (pH=3) and the suspension was extracted with ethyl acetate. The organic extracts were combined, washed with water, dried over sodium sulfate and concentrated under reduced pressure. The residue was chromatographed on silica gel with toluene-ethyl acetate 9:1 and yielded 4-tert-butyl-N-[6-chloro-5-(2-methoxyphenoxy)-2-(thiophen-2-yl)-pyrimidin-4-yl]-benzenesulphonamide as a white foam.

According to the analysis of related databases, 6292-59-7, the application of this compound in the production field has become more and more popular.

Reference:
Patent; Hoffmann-La Roche Inc.; US5292740; (1994); A;,
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. 703-12-8, name is 4-Bromo-N-methylbenzenesulfonamide belongs to amides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below. Safety of 4-Bromo-N-methylbenzenesulfonamide

4-Bromo-N-methylbenzenesulfonamide (100 mg, 0.40 mmol), 5-cyano-1-methyl-1H-pyrrol-2-ylboronic acid (72 mg, 0.48 mmol), potassium fluoride (76 mg, 1.3 mmol), and tris(dibenzylideneacetone)dipalladium(0) (10 mg, 0.01 mmol) were placed in an oven dried flask under nitrogen and dry THF (1.0 mL) was added. Tri-t-butylphosphine (60 muL, 0.02 mmol, 10 wt % in hexane) was added and the reaction was stirred for 16 hours. The reaction mixture was filtered through silica and rinsed with ethyl acetate. The solvent was concentrated in vacuo to provide the crude product. The crude product was pre-adsorbed onto the Celite reagent and purified via Isco chromatography (the Redisep column, silica, gradient 5-50% ethyl acetate in hexane) to afford 4-(5-cyano-1-methyl-1H-pyrrol-2-yl)-N-methylbenzenesulfonamide (28 mg, 25%). MS (ESI) m/z 275. HPLC purity 100.0% at 210-370 nm, 9.0 min.; the Xterra RP18 column, 3.5mu, 150*4.6 mm column, 1.2 mL/min., 85/15-5/95 (ammonium formate buffer pH=3.5/ACN+MeOH) for 10 min., hold 4 min.

The synthetic route of 703-12-8 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Wyeth; US2008/221201; (2008); A1;,
Amide – Wikipedia,
Amide – an overview | ScienceDirect Topics

Synthetic Route of 121-30-2, These common heterocyclic compound, 121-30-2, name is 4-Amino-6-chlorobenzene-1,3-disulfonamide, 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 aminoacetaldehyde dimethylacetal (2.18 mL, 2.13 g, 20.2 mmol) in EtOAc (25 mL) at 0 C. was added dropwise a solution of HCl in ether (13 mL, 2N solution in ether). The mixture was stirred at 0 C. for 5 minutes. To this solution, 4-chloro-6-aminobenzene-1,3-disulfonamide (Aldrich, 5.8 g, 20.3 mmol) in diethylene glycol dimethylether (30 mL) was added. The reaction mixture was then heated at 60-90 C. for 1 hour. The solvent was decanted and the solid was dissolved in water. An aqueous solution of Na2CO3 (10%) was added to adjust the pH 7-8, extracted with EtOAc, dried over Na2SO4, filtered and the solvent was evaporated. The crude material was chromatographed on silica gel eluting with CH2Cl2:EtOAc:MeOH (1:1:0.2 to 1:1:1) to give the title compound (3 g, 53% yield) as a white solid: mp 157-160 C. 1H NMR (400 MHz, d6-DMSO) delta 7.97 (s, 1H), 7.05 (s, 1H), 5.65-4.70 (m, 1H), 2.88-2.96 (m, 1H), 2.77-2.84 (m, 1H); 13C NMR (100 MHz, d6-DMSO) delta 147.1, 134.8, 128.4, 125.9, 118.7, 117.6, 68.1, 44.9. Mass spectrum (API-TIS) m/z 325 (M-H), 327 (MH+); Anal. calcd for C8H11ClN4O4S20: C, 30.06; H, 3.54; N, 16.70. Found: C, 30.26; H, 3.40; N, 16.38.

Statistics shows that 4-Amino-6-chlorobenzene-1,3-disulfonamide is playing an increasingly important role. we look forward to future research findings about 121-30-2.

Reference:
Patent; NitroMed, Inc.; US2006/189603; (2006); 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. 121492-06-6, name is N-Boc-(2-Aminoethyl)-N-methylamine, A new synthetic method of this compound is introduced below., name: N-Boc-(2-Aminoethyl)-N-methylamine

Step 1 [0216] A solution of N-Boc-N-methylethylenediamine (1 g, 5.74 mmol) and sulfamide (1.1 g, 11.48 mmol) in dioxane (20 mL) was stirred at reflux under N2 atmosphere (monitored by TLC). The mixture was then filtered to remove the insoluble material and the filtrate was concentrated under reduced pressure and treated with ethyl acetate. The insoluble material was again removed by filtration and the filtrate concentrated under reduced pressure to give the desired product in 96% yield.

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; FOB SYNTHESIS; WO2005/123066; (2005); 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. 354-38-1, name is 2,2,2-Trifluoroacetamide, This compound has unique chemical properties. The synthetic route is as follows., Application In Synthesis of 2,2,2-Trifluoroacetamide

Intermediate 186 (0.43 g, 1.22 mmol) was dissolved in DCM (20 mL) and 2,2,2- trifluroacetamide (0.28 g, 2.49 mmol), magnesium oxide (0.21 g, 5.1 mmol), rhodium(II) acetate dimer (0.028 g, 0.064 mmol) and iodobenzene I,I-diacetate (0.53 g, 1.65 mmol) were added. After 18 h at r.t. the pink solution was filtered through a pad of celite and concentrated in vacuo. The residue was purified by column chromatography (Si02, 20- 60% EtOAc:DCM) to yield the title compound (0.39 g, 90%). HPLC-MS : MH+ mlz 431 , RT 2.00 minutes

According to the analysis of related databases, 354-38-1, the application of this compound in the production field has become more and more popular.

Reference:
Patent; UCB BIOPHARMA SPRL; BRACE, Gareth Neil; CHOVATIA, Prafulkumar Tulshibhai; FOULKES, Gregory; JOHNSON, James Andrew; JONES, Severine Danielle; KROEPLIEN, Boris; LECOMTE, Fabien Claude; LOKE, Pui Leng; LOWE, Martin Alexander; MANDAL, Ajay; NORMAN, Timothy John; PALMER, Christopher Francis; PEREZ-FUERTES, Yolanda; PORTER, John Robert; SMYTH, Donald; TRANI, Giancarlo; UDDIN, Muhammed; ZHU, Zhaoning; (207 pag.)WO2016/198400; (2016); A1;,
Amide – Wikipedia,
Amide – an overview | ScienceDirect Topics