Month: August 2021

Application of 2896-98-2, 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. 2896-98-2, name is Tetrahydro-1,4-thiazepan-5-one, This compound has unique chemical properties. The synthetic route is as follows.

(Ref: J. Org. Chem. 1960, 25, 1953-1956.) To a stirred solution of 1,4- thiazepan-5-one (9.16 g, 70 mmol) in THF (271 mL) at 0 0C is added dropwise over20 min LAH (IM in THF, 70 mL, 70 mol). The reaction mixture is stirred at 0 0C for 10 min and then warmed to RT, stirring is continued for 2 h. The reaction mixture is quenched with careful successive addition of H2O (2.5 mL), 5N aqeous NaOH (2.5 mL) and H2O (9 mL). A thick gel like precipitate formed. The reaction mixture is filtered through a small pad of Celite, and the filter cake is washed with ether (300 mL). The filtrate is concentrated to afford the title compound as an oil, which is used immediately in the next reaction. 1H NMR (400 MHz, DMSO) delta 2.89 (t, 2H), 2.84 (t, 2H), 2.69 (t, 2H), 2.59 (t,2H), 1.78 (m, 2H).

The chemical industry reduces the impact on the environment during synthesis Tetrahydro-1,4-thiazepan-5-one. I believe this compound will play a more active role in future production and life.

Reference:
Patent; PHARMACIA & UPJOHN COMPANY LLC; WO2006/56875; (2006); A1;,
Amide – Wikipedia,
Amide – an overview | ScienceDirect Topics

Adding a certain compound to certain chemical reactions, such as: 685-91-6, name is N,N-Diethylacetamide, 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 685-91-6, HPLC of Formula: C6H13NO

General procedure: To the solution of 0.50 g (2.0 mmol) 2-bromo-3-aminobenzanthrone (1) in 2-3ml of appropriate amides, the phosphorusoxychloride (0.2 ml, 2.1 mmol) was added dropwise under stirring.The resulting mixture was heated for 3 h at 90-100 C. After cooling tothe ambient temperature, the crude product that precipitated onpouring into 50 ml of 2% NaOH water solution was filtered, washedwith water, and dried.

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

Reference:
Article; Kirilova; Puckins; Romanovska; Fleisher; Belyakov; Spectrochimica Acta Part A: Molecular and Biomolecular Spectroscopy; vol. 202; (2018); p. 41 – 49;,
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. 869640-41-5, name is 7-Benzyl-5,6,7,8-tetrahydro-1,7-naphthyridin-2(1H)-one, A new synthetic method of this compound is introduced below., Recommanded Product: 7-Benzyl-5,6,7,8-tetrahydro-1,7-naphthyridin-2(1H)-one

To a solution of the product of preparation 26 (620mg, 2.22mmol) in toluene (30mL) was added the product of preparation 4 (344mg, 2.64mmol), tri-n-butylphosphine (0.66mL, 2.64mmol) and 1,1′-azobis(N,N-dimethylformamide) (458mg, 2.24mmol) and the reaction mixture was stirred at 85C for 18 hours. The solvent was then evaporated under reduced pressure and the residue was purified by column chromatography on silica gel, eluting with dichloromethane:methanol:0.88 ammonia, 90:10:0.5. The crude product was dissolved in dichloromethane (20mL), washed with 2M sodium hydroxide, dried over magnesium sulfate and concentrated in vacuo to afford the title compound in 33% yield, 255mg. 1HNMR(CDCl3, 400MHz) delta: 1.79(m, 4H), 1.94(m, 2H), 2.55(m, 4H), 2.61(m, 2H), 2.76(m, 4H) 3.51 (s, 2H), 3.70(s, 2H), 4.21 (m, 2H), 6.55(d, 1H), 7.25-7.41 (brm, 6H) MS APCl+ m/z 352 [MH]+

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; Pfizer Limited; EP1595881; (2005); A1;,
Amide – Wikipedia,
Amide – an overview | ScienceDirect Topics

Some common heterocyclic compound, 598-55-0, name is Methyl carbamate, molecular formula is C2H5NO2, 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. category: amides-buliding-blocks

General procedure: To a well-ground mixture of beta-naphthol (0.288 g, 2 mmol), aldehyde (2 mmol) and amide derivatives (2.4 mmol) in a 10 mL round-bottomed flask connected to a reflux condenser, was added TrCl (0.055 g, 0.2 mmol), and the resulting mixture was stirred in an oil-bath (70 C) for the times reported in Table 2. Afterward, petroleum ether (20 mL) was added to the reaction mixture, refluxed, and stirred for 3 min, and filtered (TrCl is soluble in petroleum ether; however, the products are insoluble in this solvent). The filtrate containing the catalyst was washed two times with 20 mL of 40% (w/v) solution of NaHSO3 in H2O/EtOH (4:1) to extract the unreacted aldehyde dissolved in the petroleum ether. The organic layer was separated and dried with CaCl2; the solvent was evaporated to give pure recycled TrCl. The solid residue was recrystallized from EtOH (95%) to give the pure product (compounds 1a-m, 2a-d, and 3a-e).

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 598-55-0, its application will become more common.

Reference:
Article; Khazaei, Ardeshir; Zolfigol, Mohammad Ali; Moosavi-Zare, Ahmad Reza; Abi, Fereshteh; Zare, Abdolkarim; Kaveh, Hamideh; Khakyzadeh, Vahid; Kazem-Rostami, Masoud; Parhami, Abolfath; Torabi-Monfared, Hossein; Tetrahedron; vol. 69; 1; (2013); p. 212 – 218;,
Amide – Wikipedia,
Amide – an overview | ScienceDirect Topics

Reference of 147356-78-3, 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. 147356-78-3, name is N-Methoxy-N-methylcyclopropanecarboxamide belongs to amides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

To a solution of (5S,7S)-2-bromo-7-fluoro-5-(2-fluorophenyl)-6,7-dihydro-5H-pyrrolo[l,2- b][l,2,4]triazole (500 mg, 1.67 mmol) and N-methoxy-N-methyl-cyclopropanecarboxamide (430 mg, 3.33 mmol) in tetrahydrofuran (10 mL) was added isopropylmagnesium chloride (2.0 M in tetrahydrofuran, 4.2 mL, 8.4 mmol) at 0 C under nitrogen atmosphere. The reaction mixture was stirred at 0C for 2 h and then quenched by addition of water (10 mL). The mixture was extracted with ether acetate (3 x 10 mL). The combined organic layers were dried over sodium sulfate and concentrated under reduced pressure to afford crude cyclopropyl-[(5S,7S)-7-fluoro-5-(2- fluorophenyl)-6,7-dihydro-5H-pyrrolo[l,2-b][l,2,4]triazol-2-yl]methanone (350 mg, 72%) as green oil.

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

Reference:
Patent; F. HOFFMANN-LA ROCHE AG; GENENTECH, INC.; CHEN, Huifen; HAMILTON, Gregory; PATEL, Snahel; ZHAO, Guiling; DANIELS, Blake; STIVALA, Craig; (208 pag.)WO2019/72942; (2019); A1;,
Amide – Wikipedia,
Amide – an overview | ScienceDirect Topics

Related Products of 67442-07-3, 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.

4-Iodo-l-(4-methoxybenzyl)-lH-pyrazole (8.1 g, 26 mmol) was dissolved in THF (50 mL) and cooled in an ice bath. Isopropylmagnesium chloride (2.9 M, 8.9 mL, 26 mmol) was added slowly. The reaction mixture was stirred for 10 min, and then 2-chloro-N-methoxy-N- methylacetamide (3.5 g, 26 mmol) dissolved in THF (15 mL) was added slowly by syringe. The reaction mixture was warmed to ambient temperature and stirred for 1 h. The reaction mixture was partitioned between EtOAc and IN HC1, and the organic layer was dried over sodium sulfate, filtered, and concentrated to afford the crude title compound (7.1 g, 104percent yield) as an amber oil that slowly solidified.

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

Reference:
Patent; ANDREWS, Steven W.; BLAKE, James F.; HAAS, Julia; JIANG, Yutong; KOLAKOWSKI, Gabrielle R.; MORENO, David A.; REN, Li; WALLS, Shane M.; (421 pag.)WO2018/136661; (2018); A1;,
Amide – Wikipedia,
Amide – an overview | ScienceDirect Topics

Application of 869494-16-6, These common heterocyclic compound, 869494-16-6, name is tert-Butyl 3,6-diazabicyclo[3.1.1]heptane-6-carboxylate, 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.

In a microwave vial a solution of 3 -chloro-4-(6-fluoropyridin-3 -yl)-6-( i-methyl-i Hpyrazol-4-yl)pyrazolo[i,5-a]pyridine (Intermediate P9; 5 mg, 0.015 mmol) and tert-butyl 3,6- diazabicyclo[3.i.i]heptane-6-carboxylate (9.1 mg, 0.046 mmol) in DMSO (0.2 mL) was subjected to microwave irradiation at 130 °C for 5 h and then at 150 °C for 6 h. The reaction mixture was cooled to ambient temperature and then directly purified by reverse phase chromatography (5-95percent ACN/water) to afford the title compound (2.6 mg, 34percent yield). ?H NIVIR (CDC13) 8.51 (d, 1H), 8.34 (d, 1H), 7.88 (s, 1H), 7.76 (s, 1H), 7.65 (m, 2H), 7.12 (d, 1H), 6.62(d, 1H), 4.33 (m, 2H), 4.20 (m, 2H), 3.98 (s, 3H), 3.55 (m, 2H), 1.45 (d, 2H), 1.38 (s, 9H).

Statistics shows that tert-Butyl 3,6-diazabicyclo[3.1.1]heptane-6-carboxylate is playing an increasingly important role. we look forward to future research findings about 869494-16-6.

Reference:
Patent; ARRAY BIOPHARMA, INC.; ANDREWS, Steven W.; BLAKE, James F.; CHICARELLI, Mark J.; GOLOS, Adam; HAAS, Julia; JIANG, Yutong; KOLAKOWSKI, Gabrielle R.; (594 pag.)WO2017/11776; (2017); A1;,
Amide – Wikipedia,
Amide – an overview | ScienceDirect Topics

Adding a certain compound to certain chemical reactions, such as: 25625-57-4, name is 2-Bromo-N-(3-(trifluoromethyl)phenyl)acetamide, 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 25625-57-4, SDS of cas: 25625-57-4

General procedure: Urea linked alkynes 2(a-c) (1.0 mmol), 2-bromo-N-phenylacetamides3(a-f) (1.0 mmol) were dissolved in dimethylformamide(4 mL) in a round bottom flask. Sodium azide (3.0 mmol) in water (2 mL) copper sulphate (0.02 mmol) in water (2 mL) wereadded to the reaction mixture followed by addition of sodiumascorbate (0.02 mmol) and the mixture was stirred at 40 C for2e3 h. After completion of the reaction, reaction mixture wasfiltered and the solid obtained was washed with ice cold water andsmall amount of ethyl acetate to yield triazole hybrids 4(a-r).

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, 2-Bromo-N-(3-(trifluoromethyl)phenyl)acetamide, other downstream synthetic routes, hurry up and to see.

Reference:
Article; Kumar, Anil; Kumar, Ashwani; Lal, Kashmiri; Poonia, Nisha; Rani, Poonam; Journal of Molecular Structure; vol. 1215; (2020);,
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. 86499-96-9, name is 3-Bromo-4,5-dihydro-1H-benzo[b]azepin-2(3H)-one, A new synthetic method of this compound is introduced below., Quality Control of 3-Bromo-4,5-dihydro-1H-benzo[b]azepin-2(3H)-one

To a suspension of 3-bromo-1,3,4,5-tetrahydro-1-benzazepin-2-one (9.56 g, 40 mmol) in acetic acid (40 mL) was added bromine (12.8 g, 80 mmol) dropwise. The resulting mixture was stirred at rt for 14 h. The resulting precipitate was collected by filtration, washed with HOAc, and dried to give 72A as a white solid (11.54 g, 91percent). LC/MS m/z 317 (M+H)+.

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; Bristol-Myers Squibb Company; US2007/93470; (2007); A1;,
Amide – Wikipedia,
Amide – an overview | ScienceDirect Topics

Synthetic Route of 337463-88-4, These common heterocyclic compound, 337463-88-4, name is 6-Bromo-2H-pyrido[3,2-b][1,4]oxazin-3(4H)-one, 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.

6-Bromo-4/-/-pyrido[3,2-b][1 ,4]oxazin-3-one (6.0 g, 26.3 mmole) and trans-2- phenylvinylboronic acid (3.9 g, 26.3 mmole) were dissolved in 1 ,4-dioxane (150 mL) and the solution was degassed with argon. (PhbetaP^Pd (230 mg, 0.2 mmole) was added, followed by a solution of potassium carbonate (6.9 g, 50 mmole) in H2O (20 mL). The reaction was heated at reflux under argon overnight, then was cooled to room temperature and diluted with EtOAc (200 mL). The solution was washed sequentially with H2O and brine, dried (Na2SO4), and concentrated in vacuo. The solid residue was purified by flash chromatography on silica gel (5-10% EtOAc/CHCl3) to afford a solid (2.5 g, 38%): LCMS(ES) m/z253.0 (M + H)+.

Statistics shows that 6-Bromo-2H-pyrido[3,2-b][1,4]oxazin-3(4H)-one is playing an increasingly important role. we look forward to future research findings about 337463-88-4.

Reference:
Patent; GLAXO GROUP LIMITED; WO2006/81182; (2006); A2;,
Amide – Wikipedia,
Amide – an overview | ScienceDirect Topics