Continuously updated synthesis method about 72594-62-8

At the same time, in my other blogs, there are other synthetic methods of this type of compound, tert-Butyl naphthalen-1-ylcarbamate, and friends who are interested can also refer to it.

Adding a certain compound to certain chemical reactions, such as: 72594-62-8, name is tert-Butyl naphthalen-1-ylcarbamate, 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 72594-62-8, Product Details of 72594-62-8

General procedure: Under argon, to a solution of N-Boc-1-naphthylamine (1a) or 1-naphthyl-N-pivalamide (1b) (2.2 mmol) in dry Et2O (15 mL) at -20 C, t-BuLi in pentane (4.6 mmol) was added dropwise. The reaction mixture was stirred at this temperature for 2 h. Next, to the solution of lithiated species was added dropwise at -20 C, a solution of an appropriate electrophile (ethyl chloroformate, 2.2 mmol) in dry Et2O (10 mL). Then, the mixture was allowed to warm to room temperature and was stirred under these conditions for 2 h. After this time, to the reaction mixture a saturated solution of NH4Cl (20 mL) was added and was stirred for 0.5 h. The water layer was separated and extracted subsequently with Et2O (3¡Á20 mL). The organic phase was dried over MgSO4 and concentrated till dryness. The crude material was separated by flash chromatography.

At the same time, in my other blogs, there are other synthetic methods of this type of compound, tert-Butyl naphthalen-1-ylcarbamate, and friends who are interested can also refer to it.

Reference:
Article; Nowak, Monika; Malinowski, Zbigniew; Jo?wiak, Andrzej; Fornal, Emilia; B?aszczyk, Alina; Kontek, Renata; Tetrahedron; vol. 70; 34; (2014); p. 5153 – 5160;,
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Extended knowledge of 193751-54-1

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.

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. 193751-54-1, name is tert-Butyl cyclopent-3-en-1-ylcarbamate, A new synthetic method of this compound is introduced below., category: amides-buliding-blocks

(0243) To a stirred suspension of LiAlH4 (3.74 g, 0.09852 mol) in 200 ml anhydrous THF in a two neck RBF (1 L), was added a solution of 514 (10 g, 0.04926 mol) in 70 mL of THF slowly at 0 C. under nitrogen atmosphere. After complete addition, reaction mixture was warmed to room temperature and then heated to reflux for 4 h. Progress of the reaction was monitored by TLC. After completion of reaction (by TLC) the mixture was cooled to 0 C. and quenched with careful addition of saturated Na2SO4 solution. Reaction mixture was stirred for 4 h at room temperature and filtered off. Residue was washed well with THF. The filtrate and washings were mixed and diluted with 400 mL dioxane and 26 mL conc. HCl and stirred for 20 minutes at room temperature. The volatilities were stripped off under vacuum to furnish the hydrochloride salt of 515 as a white solid. Yield: 7.12 g 1H-NMR (DMSO, 400 MHz): delta=9.34 (broad, 2H), 5.68 (s, 2H), 3.74 (m, 1H), 2.66-2.60 (m, 2H), 2.50-2.45 (m, 5H). (0244) Synthesis of 516:

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; Alnylam Pharmaceuticals, Inc.; Novobrantseva, Tatiana; Bettencourt, Brian; Milstein, Stuart; Borodovsky, Anna; US9127275; (2015); B2;,
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Discovery of 85006-25-3

Chemical properties determine the actual use. Each compound has specific chemical properties and uses. We look forward to more synthetic routes in the future to expand reaction routes of 85006-25-3.

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. 85006-25-3, name is tert-Butyl (tert-butoxycarbonyl)oxycarbamate, This compound has unique chemical properties. The synthetic route is as follows., Recommanded Product: 85006-25-3

Reagent and conditions: (a) tert-butyl (tert-butoxycarbonyl) oxycarbamate, 1N NaOH, TBAB, DCM; (b) TFA, DCM; (c) 2, 2-dimethylbutanoyl chloride, aq. NaHCO 3, THF, H 2O. Tert-butyl (tert-butoxycarbonyl) oxycarbamate (400 mg) and 1- (bromomethyl-d2) benzene-2, 3, 4, 5, 6-d5 (100mg) were dissolved in CH 2Cl 2 (4 ml) . The mixture was added 1M NaOH (2 ml) and tetrabutylammonium bromide (25.2 mg) , and stirred at room temperature for overnight. The resulting mixture was washed with water and dried with Na 2SO 4, concentrated in vacuo and purification by silica gel chromatography to give tert-butyl ( (tert-butoxycarbonyl) oxy) ( (phenyl- d5) methyl-d2) carbamate (510 mg, 99%) . 1HNMR (400 MHz, CDCl 3) delta 1.46 (s, 9H) , 1.44 (s, 9H) .

Chemical properties determine the actual use. Each compound has specific chemical properties and uses. We look forward to more synthetic routes in the future to expand reaction routes of 85006-25-3.

Reference:
Patent; SU, Yaning; SIRONAX LTD; ZHANG, Zhiyuan; YANG, Yi; WANG, Guozheng; LIU, Wendong; MA, Yongfen; REN, Yan; (74 pag.)WO2020/103859; (2020); A1;,
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Some tips on 16695-22-0

The synthetic route of 16695-22-0 has been constantly updated, and we look forward to future research findings.

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. 16695-22-0, name is (Tosylazanediyl)bis(ethane-2,1-diyl) bis(4-methylbenzenesulfonate), A new synthetic method of this compound is introduced below., Quality Control of (Tosylazanediyl)bis(ethane-2,1-diyl) bis(4-methylbenzenesulfonate)

Synthesis of Intermediate XVI. To a solution of Tritosylate XV (1 g, 0.00176 moles, 1 eq) in 6 ml of DMF was added NaBr (0.93 g, 0.009 moles, 5 eq). The resulting suspension was stirred in an oil bath at 120 C. for 4 h. After cooling to room temperature, the reaction mixture was concentrated to about 2 ml. The viscous milky product was poured into rapidly stirred mixture of ice-water (30 ml) and extracted with ethyl acetate (30 ml). The organic phase was dried (Na2SO4) and concentrated under reduced pressure. The crude product was purified by column chromatography (silica gel, 60-120 mess, 10% ethyl acetate in hexane) to leave the product XVI as a pale yellow liquid (0.34 g, 51%) 1H NMR (400 MHz, CDCl3) 2.41 (s, 3H), 3.44 (s, 8H), 7.38 (d, 4H), 7.76 (d, 4H)

The synthetic route of 16695-22-0 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Salituro, Francesco G.; Saunders, Jeffrey; Yan, Shunqi; US2012/172349; (2012); A1;,
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Introduction of a new synthetic route about 18807-71-1

The synthetic route of Benzyl N-(2-aminoethyl)carbamate hydrochloride has been constantly updated, and we look forward to future research findings.

Application of 18807-71-1, 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. 18807-71-1, name is Benzyl N-(2-aminoethyl)carbamate hydrochloride belongs to amides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

EXAMPLE 178; 4-[7-(2-Oxo-imidazolidin-1-yl)-quinazolin-4-yl]-piperidine-1-carboxylic acid (4-pyrrolidin-1-yl-phenyl)-amide; a. 4-[7-(2-Oxo-imidazolidin-1-yl)-quinazolin-4-yl]-piperidine-1-carboxylic acid tert-butyl ester; To a mixture of 4-(7-fluoro-quinazolin-4-yl)-piperidine-1-carboxylic acid tert-butyl ester (458 mg, 1.38 mmol), which was prepared as described in Example 65b, and (2-amino-ethyl)-carbamic acid benzyl ester hydrochloride (446 mg, 1.93 mmol) in DMSO (1.0 mL) was added K2CO3 (1.52 g, 11.04 mmol). The mixture was stirred at 115 C. overnight and subsequently partitioned between EtOAc and water. The combined organic extracts were washed with brine, dried over Na2SO4 and evaporated. The residue was purified by flash column chromatography on silica gel (EtOAc as eluent) to afford the desired product as a white solid (400 mg, 73%). 1H NMR (CDCl3) delta 9.13 (s, 1H), 8.69 (dd, J=9.40 and 2.35 Hz, 1H), 8.08 (d, J=9.53 Hz, 1H), 7.42 (d, J=2.33 Hz, 1H), 5.25 (br, 1H), 4.31 (m, 2H), 4.09 (t, J=8.21 Hz, 2H), 3.69 (t, J=8.14 Hz, 2H), 3.63 (m, 1H), 2.95 (m, 2H), 1.77-2.04 (4H), 1.48 (s, 9H). Calcd for C21H28N5O3 (MH+) 398.3, found 398.3.

The synthetic route of Benzyl N-(2-aminoethyl)carbamate hydrochloride has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Baindur, Nand; Gaul, Michael David; Kreutter, Kevin Douglas; Baumann, Christian Andrew; Kim, Alexander J.; Xu, Guozhang; Tuman, Robert W.; Johnson, Dana L.; US2006/281772; (2006); A1;,
Amide – Wikipedia,
Amide – an overview | ScienceDirect Topics

The important role of 1103234-56-5

Chemical properties determine the actual use. Each compound has specific chemical properties and uses. We look forward to more synthetic routes in the future to expand reaction routes of 1103234-56-5.

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. 1103234-56-5, name is 2,6-Difluoro-3-(propylsulfonamido)benzoic acid, This compound has unique chemical properties. The synthetic route is as follows., Application In Synthesis of 2,6-Difluoro-3-(propylsulfonamido)benzoic acid

Example GN-(3 -Amino-2,4-difluorophenyl)propane- 1 -sulfonamideTo a solution of 2,6-difluoro-3-(propylsulfonamido)benzoic acid (4.078 g, 14.6 mmol) inTHF (60 mL) was added triethylamine (4.68 mL, 33.59 mmol) and diphenylphosphonic azide (3.73 mL, 16.79 mmol). The reaction mixture was stirred at room temperature for 3 hours and then warmed to 80 0C for 2 hours. Water (10 mL) was added, and the mixture stirred at 80 0C for 15 hours. The reaction mixture was diluted with 300 mL of EtOAc, and the organic layer was washed with saturated aq. NaHCO3 solution and brine. The solvent was removed under reduced pressure and the residual purified via silica gel column chromatography eluting with 30/70 EtOAc/hexane to obtain 2.03 g (55%) of the title compound. 1H NMR (400 MHz, DMSO- d6) delta 9.32 (s, IH), 6.90-6.80 (m, IH), 6.51 (td, J=8.7, 5.5 Hz, IH), 5.28 (s, 2H), 3.05-2.96 (m, 2H), 1.82-1.64 (m, 2H), 1.01-0.90 (m, 3H). LC/MS: m/z 251.1 [M+l].

Chemical properties determine the actual use. Each compound has specific chemical properties and uses. We look forward to more synthetic routes in the future to expand reaction routes of 1103234-56-5.

Reference:
Patent; ARRAY BIOPHARMA INC.; GENENTECH, INC.; ALIAGAS, Ignacio; GRADL, Stefan; GUNZNER, Janet; LEE, Wendy; MATHIEU, Simon; RUDOLPH, Joachim; WEN, Zhaoyang; ZHAO, Guiling; BUCKMELTER, Alexandre J.; GRINA, Jonas; HANSEN, Joshua D.; LAIRD, Ellen; MORENO, David; REN, Li; WENGLOWSKY, Steven Mark; WO2011/25938; (2011); A2;,
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Sources of common compounds: 86-86-2

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.

Adding a certain compound to certain chemical reactions, such as: 86-86-2, name is 1-Naphthaleneacetamide, 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 86-86-2, COA of Formula: C12H11NO

General procedure: A mixture of the amide (1, 1 mmol), alcohol (15 mL), and pulverized potassium bisulfate (1.1 g, 8 mmol) was refluxed for the specified time. The alcohol was removed in vacuo and the residue was triturated with hexanes (or other appropriate solvent such as DCM or ethyl acetate to dissolve the product). Removal of hexanes in vacuo provided the following pure products

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; Sattenapally, Narsimha; Sharma, Jhanvi; Hou, Yuqing; Arkivoc; vol. 2018; 5; (2018); p. 174 – 183;,
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Sources of common compounds: 89979-12-4

According to the analysis of related databases, 89979-12-4, the application of this compound in the production field has become more and more popular.

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. 89979-12-4, name is 5-Chloro-2-(methylsulfonamido)benzoic acid, This compound has unique chemical properties. The synthetic route is as follows., name: 5-Chloro-2-(methylsulfonamido)benzoic acid

Mixed 5-chloro-2-(methylsulfonamido)benzoic acid (28mg, 0.109mmol) with HATU (42mg, 0.109mmol) and dissolved in anhydrous DMF (300uL). Stirred for Ihr. Dissolved hydrogenation product in anhydrous DMF (300uL) and added to the reaction. Added TEA (30uL, 0.218mmol).Stirred for 12 hrs. Diluted with acetonitrile and purified with Prep HPLC to give compound 40 (22mg, 32% yield).1H NMR (400MHz, CD3OD): delta 7.49 (m, 3H), 6.26 (m, 1H), 6.08 (m, 1H), 4.78 (m, 1H), 4.57 (m, 2H), 4.14 (m, 2H), 3.47-3.34 (m, 2H), 3.01 (m, 4H), 2.76 (s, 3H), 2.40-2.05 (m, 2H), 1.73- 1.50 (m, 4H). LC/MS (m/z): 519.2 [M+H]+

According to the analysis of related databases, 89979-12-4, the application of this compound in the production field has become more and more popular.

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;,
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Continuously updated synthesis method about 5466-88-6

The synthetic route of 5466-88-6 has been constantly updated, and we look forward to future research findings.

Reference of 5466-88-6, A common heterocyclic compound, 5466-88-6, name is 2H-1,4-Benzoxazin-3(4H)-one, molecular formula is C8H7NO2, 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.

4-(4-Bromobutan-1-yl)-3,4-dihydro-2H-1,4-benzoxazin-3(4H)-one from 3,4-dihydro-2H-1,4-benzoxazin-3(4H)-one and 1,4-dibromobutane

The synthetic route of 5466-88-6 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; H. Lundbeck A/S; US2003/191133; (2003); A1;,
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Analyzing the synthesis route of 402-46-0

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

These common heterocyclic compound, 402-46-0, name is 4-Fluorobenzenesulfonamide, 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. Quality Control of 4-Fluorobenzenesulfonamide

Example 44; 4-{2-[4-(4-Sulfamoylphcnyl)pipcrazin-l-yl]cthyl}pipcridinc-l-carboxylic acid tert-butyl ester hydrochloride; EPO A mixture of 4-fluorobenzenesulfonamide (1.00 g, 5.71 mmol) and piperazine (2.46 g, 28.54 mmol) in water (12 mL) was heated at 1000C for 2Oh. The resulting precipitate was collected filtration and washed with water and toluene to give 4-piperazin-l- ylbenzenesulfonamide: RT = 0.49 min; m/z (ES+) = 242.13 [M+H]+. A solution of 4-piperazin- 1-ylbenzenesulfonamide (0.46 g, 1.89 mmol) and 4-(2-oxoethyl)piperidine-l-carboxylic acid tert-butyl ester (0.43 g, 1.89 mmol) in DCM (50 mL) and THF (7 mL) with molecular sieves (0.90 g) was stirred under argon at rt for Ih. Sodium acetoxyborohydride (0.52 g, 2.46 mmol) was added and the reaction mixture was stirred for a further 2.5h. The reaction mixture was quenched with saturated NaHCO3 solution and extracted with EtOAc. The organic extracts were washed with brine, dried (MgSO4) and the solvent was removed under vacuum. The resulting solid was purified by recrystallisation (EtOAc) then dissolved in THF and 1 M HCl in dioxane (0.95 equivalents), the solvent was removed under vacuum and the resulting solid was washed with Et2O to afford the title compound: RT = 2.51 min; m/z (ES+) = 453.33 [M+H]+.

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

Reference:
Patent; PROSIDION LIMITED; WO2007/3964; (2007); A1;,
Amide – Wikipedia,
Amide – an overview | ScienceDirect Topics