7-Sep-21 News Continuously updated synthesis method about 2886-65-9

The synthetic route of 2886-65-9 has been constantly updated, and we look forward to future research findings.

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. 2886-65-9, name is 7-Chloro-5-(2-fluorophenyl)-1H-benzo[e][1,4]diazepin-2(3H)-one belongs to amides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below. name: 7-Chloro-5-(2-fluorophenyl)-1H-benzo[e][1,4]diazepin-2(3H)-one

EXAMPLE 3 Preparation of 10-chloro-11b-(2-fluorophenyl)-2,3,5,11b-tetrahydrooxazolo[3,2-d] [1,4]benzodiazepin-6-(7H)-one SPC17 To 15 g. (51.9 mmole) of 7-chloro-5-(2-fluorophenyl)-1,3-dihydro-2H-1,4-benzodiazepin-2-one in 150 ml. of dry benzene, 9 g. (67.7 mmole) of aluminum chloride was added and stirring was continued 15 minutes. The reaction mixture was cooled in an ice bath and 8.8 g. (0.2 mole) of ethylene oxide was added dropwise. After 18 hours of stirring at room temperature, the reaction mixture was heated to 40 for 1 hour and then cooled to room temperature and treated with 5 g. (37.6 mmole) of aluminum chloride, followed by 4.4 g. (0.1 mole) of ethylene oxide. The reaction mixture was heated 4 hours at 45-50 and then evaporated to dryness. ethylene chloride, ice and ammonium hydroxide were added and the solid removed by filtration. The filtrate was separated and the organic phase reduced to dryness in vacuo. The residue was dissolved in dilute hydrochloric acid and the pH of the solution adjusted to 5 with ammonium hydroxide. The acidic solution was washed with ether, made basic and extracted with methylene chloride. The organic phase was washed with brine, dried and evaporated to dryness. Recrystallization from methylene chloride-hexane gave the above-titled product as colorless rods, m.p. 183-184.

The synthetic route of 2886-65-9 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Hoffmann-La Roche Inc.; US3965151; (1976); A;,
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7-Sep-21 News Research on new synthetic routes about 144-80-9

The synthetic route of N-((4-Aminophenyl)sulfonyl)acetamide has been constantly updated, and we look forward to future research findings.

These common heterocyclic compound, 144-80-9, name is N-((4-Aminophenyl)sulfonyl)acetamide, 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. category: amides-buliding-blocks

The Schiff base HL1 was synthesized with a method differentfrom the one in the literature [24], by refluxing sulfacetamide(1 mmol, 0.214 g) and salicylaldehyde (1 mmol, 0.122 g) in about15 ml of methanol for 3 h at ca.70 C, in the presence of 4-5 dropsof conc. H2SO4. The solid product was collected through filtrationand finally air dried. Yield: 58%. M.P. = 215 C. Anal. Calcd. forC15H14N2O4S (%):C, 56.59; H, 4.43; N, 8.80. Found: C, 56.42; H,4.25; N, 8.75. FT-IR (KBr, cm1): mmax cm1 (KBr):1645 (s, CN),1715 (CO), 1575, 1616 (CCaromatic), 1093, 1157 (SO2) 3340(NAH). UV-vis: kmax (nm) (e, M1 cm1) (DMSO-d6): 350(40,000), 320 (41,000). 1H NMR (DMSO-d6, 400 MHz):6-8 (m, 8H), 9 (s, 1H), 10 (s, 1H), 3 (s, 3H), 11 (s, 1H).

The synthetic route of N-((4-Aminophenyl)sulfonyl)acetamide has been constantly updated, and we look forward to future research findings.

Reference:
Article; Salehi, Mehdi; Ghasemi, Fateme; Kubicki, Maciej; Asadi, Asadollah; Behzad, Mahdi; Ghasemi, Mohammad Hadi; Gholizadeh, Ahmad; Inorganica Chimica Acta; vol. 453; (2016); p. 238 – 246;,
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7-Sep-21 News The important role of 27466-83-7

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: 27466-83-7, name is 4-Bromo-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 27466-83-7, Computed Properties of C8H8BrNO

General procedure: To a dried screw-capped vial were added benzamide 2 (0.10mmol), ethyl acrylate 3 (0.15mmol), 1b (4.8mg, 0.01mmol), AgSbF6 (6.8mg, 0.02mmol), AgOAc (41.7mg, 0.25mmol), and 1,2-dichloroethane (1.0mL) under Ar atmosphere. The vial was capped and the mixture was heated at 60C for 13h with stirring. After the mixture was cooled to room temperature, saturated EDTA·2Na aqwas added following dilution with CH2Cl2. Organic layer was separated and aqueous layer was extracted with CH2Cl2 (×2). Combined organic layers were dried over Na2SO4. After filtration and evaporation, obtained crude mixture was purified by silica gel column chromatography (CH2Cl2/EtOAc) to give product3.4.1.1 _4.1.5 (E)-Ethyl 3-(5-bromo-2-(methylcarbamoyl)phenyl)acrylate (4e) A colorless solid; IR (KBr) nu 3079, 2975, 2935, 1719, 1642, 1561, 1316, 1190, 1032, 979, 862 cm-1; 1H NMR (CDCl3, 400 MHz) delta 1.32 (t, J=7.5 Hz, 3H), 3.00 (d, J=5.2 Hz, 3H), 4.23 (q, J=7.5 Hz, 2H), 5.88 (br s, 1H), 6.36 (d, J=16.0 Hz, 1H), 7.34 (d, J=8.6 Hz, 1H), 7.49 (d, J=8.6 Hz, 1H), 7.74 (s, 1H), 7.90 (d, J=16.0 Hz, 1H); 13C NMR (CDCl3, 100 MHz) delta 14.4, 27.1, 60.1, 122.1, 124.1, 124.7, 129.3, 130.1, 132.7, 134.9, 135.8, 140.5, 166.2, 168.5; HRMS (ESI): m/z calculated for [M+Na]+: 334.0049, found: 334.0050.

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; Suzuki, Yudai; Sun, Bo; Yoshino, Tatsuhiko; Kanai, Motomu; Matsunaga, Shigeki; Tetrahedron; vol. 71; 26-27; (2015); p. 4552 – 4556;,
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7-Sep-21 News Simple exploration of 194920-62-2

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. 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., Recommanded Product: 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;,
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7-Sep-2021 News New learning discoveries about 37045-73-1

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: 37045-73-1, name is 3-(Methylsulfonamido)aniline, 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 37045-73-1, Application In Synthesis of 3-(Methylsulfonamido)aniline

Under nitrogen or argon, 0.4 mmol, 0.2mmol, Ir(ppy) 3(2mg) and DMF1 ml was added to the reaction flask, followed by blue LED lights(7W) at room temperature irradiation straight trivalent iodine reagent completeconversion of the reaction. Add 10 ml of saturated Na 2CO 3Aqueous solution, andextracted three times with ethyl acetate, the organic layer was washed with water andonce with saturated brine, dried over anhydrous Na 2SO 4The organic layer was dried.Column chromatography (eluent: petroleum ether 60-90: ethyl acetate = 10: 1-5: 1) to Ethyl acetate = 10: 1-5: 1) to give the product , S; Yield 43%.Rate of 19%.

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:
Patent; Nanjing University; Zhu, ChengJian; Xie, jin; Xu, Pan; (13 pag.)CN103553857; (2016); B;,
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7-Sep-2021 News Sources of common compounds: 53844-02-3

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

Application 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;,
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9/6/21 News The important role of 120157-96-2

The synthetic route of Methyl 4-(((tert-butoxycarbonyl)amino)methyl)benzoate has been constantly updated, and we look forward to future research findings.

Application of 120157-96-2, 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. 120157-96-2, name is Methyl 4-(((tert-butoxycarbonyl)amino)methyl)benzoate belongs to amides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

(2) To a solution of the compound obtained in the above step (1) (1.5 g) in tetrahydrofuran (15 mL) was added 60 % oily dispersion of sodium hydride (407 mg) under ice-cooling and the mixture was stirred at room temperature for 30 minutes. Thereto was added dropwise ethyl iodide (2.26 mL) under ice-cooling and the mixture was stirred at 60 C for 1 hour. After cooling to room temperature, the reaction mixture was diluted with ethyl acetate (10 mL) and thereto was added water (20 mL). After stirring, the organic layer was separated and concentrated and the resultant residue was purified by a flash column chromatography on NH-silica gel (Solvent; n-hexane/ethyl acetate = 20: 1) to give methyl 4-[[N-ethyl-N-(tert-butoxycarbonyl)]aminomethyl]benzoate (929 mg, yield: 56 %) as an amorphous solid. MS(APCI)m/z; 294 [M+H]+

The synthetic route of Methyl 4-(((tert-butoxycarbonyl)amino)methyl)benzoate has been constantly updated, and we look forward to future research findings.

Reference:
Patent; TANABE SEIYAKU CO., LTD.; EP1772454; (2007); A1;,
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9/6/21 News Research on new synthetic routes about 1232365-42-2

At the same time, in my other blogs, there are other synthetic methods of this type of compound, tert-Butyl (3,3-difluoro-1-(hydroxymethyl)cyclobutyl)carbamate, and friends who are interested can also refer to it.

Adding a certain compound to certain chemical reactions, such as: 1232365-42-2, name is tert-Butyl (3,3-difluoro-1-(hydroxymethyl)cyclobutyl)carbamate, 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 1232365-42-2, SDS of cas: 1232365-42-2

Tert-Butyl N- [3,3 -difluoro- 1 -(hydroxymethyl)cyclobutyl] carbamate (900 mg, 3.79mmol) was dissolved in 25 mL of 4M HC1/dioxane at r.t. and the resulting mixture was stirredovernight. Upon completion of the reaction (monitored by 1 H NMR), the resulting mixture was concentrated under reduced pressure, the residue was treated with 20 mL of acetonitrile, and filtered. The precipitate was washed with acetonitrile and dried in vacuo to obtain (1-amino-3,3- difluorocyclobutyl)methanol hydrochloride (550.0 mg, 3.17 mmol, 83.5% yield) as whitepowder.

At the same time, in my other blogs, there are other synthetic methods of this type of compound, tert-Butyl (3,3-difluoro-1-(hydroxymethyl)cyclobutyl)carbamate, and friends who are interested can also refer to it.

Reference:
Patent; AICURIS GMBH & CO. KG; DONALD, Alastair; URBAN, Andreas; BONSMANN, Susanne; WEGERT, Anita; GREMMEN, Christiaan; SPRINGER, Jasper; (376 pag.)WO2019/86141; (2019); A1;,
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9/6/21 News The important role of 34813-49-5

The synthetic route of 34813-49-5 has been constantly updated, and we look forward to future research findings.

Electric Literature of 34813-49-5, A common heterocyclic compound, 34813-49-5, name is 2-Methylpropane-2-sulfonamide, molecular formula is C4H11NO2S, 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.

EXAMPLE 22 (RS)-S-{4-[(5-Bromo-4-{[(R)-2-hydroxy-1,2-dimethylpropyl]amino}pyrimidin-2-yl)amino]phenyl}-N-(tert-butylsulphonyl)-S-methylsulphimide Preparation of the Final ProductProduct 250 mg (0.63 mmol) of (R)-3-[{5-bromo-2-(4-methylsulphanylphenylamino) pyrimidin-4-yl)}amino]-2-methylbutan-2-ol (compound 9.1), 129 mg (0.94 mmol) of tert-butylsulphonamide, 221 mg (1.01 mmol) of iodosobenzene and 222 mg (0.63 mmol) of iron(III)acetylacetonate are weighed into a flask, and 6 ml of acetonitrile are added. The mixture is stirred at room temperature for 250 hours and then concentrated in a rotary evaporator. The remaining residue is purified by chromatography (dichloromethane/ethanol 8:2). 15 mg (0.03 mmol; yield: 4%) of the product are obtained. 1H-NMR (DMSO): 9.74 (s, 1H), 8.09 (s, 1H), 7.92 (m, 2H), 7.74 (m, 2H), 6.11 (d, 1H), 4.04 (m, 1H), 2.94 (s, 3H), 1.11 (m, 18H).

The synthetic route of 34813-49-5 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Luecking, Ulrich; Nguyen, Duy; von Bonin, Arne; von Ahsen, Oliver; Siemeister, Gerhard; Jautelat, Rolf; Doecke, Wolf-Dietrich; US2008/58358; (2008); A1;,
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9/6/21 News Continuously updated synthesis method about 148017-28-1

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.

Application of 148017-28-1, A common heterocyclic compound, 148017-28-1, name is tert-Butyl sulfamoylcarbamate, molecular formula is C5H12N2O4S, 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 {(1S,2S,4R)-2-{[tert-butyl(dimethyl)silyl]oxy}-4-[(6-{[(1R,2S)-2-methoxy-2,3-dihydro-1H-inden-1-yl]amino}pyrimidin-4-yl)oxy]cyclopentyl}methanol (105.3 mg, 0.0002168 mol), N-Boc-sulfonamide (58.9 mg, 0.000300 mol) and triphenylphosphine (85.3 mg, 0.000325 mol) in EtOAc (4.15 mL) under an atmosphere of nitrogen was added diethyl azodicarboxylate (51.9 muL, 0.000330 mol). The mixture was stirred for four hours. The solvent was removed and the orange residue was purified by flash chromatography (10 to 50% EtOAc/hexanes) to obtain 135.2 mg (94%) of the title compound.

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; Millennium Pharmaceuticals, Inc.; US2008/51404; (2008); A1;,
Amide – Wikipedia,
Amide – an overview | ScienceDirect Topics