Month: July 2021

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. 89976-75-0, name is 6-Amino-2H-1,4-benzoxazin-3(4H)-one, A new synthetic method of this compound is introduced below., Quality Control of 6-Amino-2H-1,4-benzoxazin-3(4H)-one

Example No. 26Preparation of 6- ( (5- (3 , 4 -dimethoxyphenyl) -IH-pyrazolo [4 , 3 – d] pyrimidin-7-yl) amino) -2H-benzo [b] [1 , 4] oxazin-3 (4H) -one 7-chloro-5- (3 , 4 -dimethoxyphenyl) -2- (4-methoxybenzyl) -2H- pyrazolo [4 , 3-d] pyrimidine (0.16 mmol) and 6-amino-2H- benzo [b] [1 , 4] oxazin-3 (4H) -one (0.3 mmol 2 eq. , ) were suspended in eOH (dry, 3mL) in a microwave vial (2-5mL) , HC1 in dioxane (4M, 3 drops) was added. The reaction mixture was irradiated in a microwave reactor for 5 min at 140°C. The reaction mixture was evaporated and used without further purification. The residue was dissolved in TFA (3mL) . The reaction mixture was irradiated in a microwave reactor for 5 min at 140°C. The reaction mixture was concentrated and purified by semi- preparative HPLC-MS and freeze dried from water/t-BuOH 4/1. exact mass: 418.1621 g/molHPLC-MS: analytical method Art: 2.218 min – found mass: 419 (m/z+H)

The synthetic route of 89976-75-0 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; ORIGENIS GMBH; ALMSTETTER, Michael; THORMANN, Michael; TREML, Andreas; TRAUBE, Nadine; WO2012/143144; (2012); A1;,
Amide – Wikipedia,
Amide – an overview | ScienceDirect Topics

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 114790-39-5 as follows. Formula: C12H17NO4

A solution of benzyl N-(2,2-dimethoxyethyl)carbamate (50 g, 208.9 mmol) in toluene (180 mL) is treated with solid potassium hydroxide (51.6 g, 919.69 mmol) under nitrogen. After 10 minutes, benzyltriethylammonium chloride (0.8 g, 3.1 mmol) is added. After another 10 minutes a solution of allyl bromide (33 g, 272.8 mmol) in toluene (50 mL) is added dropwise over 10 minutes. The resultant mixture is stirred at 50 C for 48hours. The mixture is cooled to room temperature and quenched with water. The organic layer is separated, washed with brine, dried over magnesium sulfate, and concentrated to dryness to give the title compound (44 g, 75%). ES/MS (mlz): 280 (M+H).

According to the analysis of related databases, 114790-39-5, the application of this compound in the production field has become more and more popular.

Reference:
Patent; ELI LILLY AND COMPANY; COATES, David Andrew; WOLFANGEL, Craig Daniel; (55 pag.)WO2016/122968; (2016); A1;,
Amide – Wikipedia,
Amide – an overview | ScienceDirect Topics

Adding a certain compound to certain chemical reactions, such as: 15910-91-5, name is 1-Methylcyclopropanecarboxamide, 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 15910-91-5, SDS of cas: 15910-91-5

Bromine (2. 87mol, 0. 056mol) was added to a solution of sodium hydroxide (13. 5g, 0. 338mol) in water (100ml) at 0-5 C. A slurry of 1- (1-methylcyclopropane) carboxamide (Method 51 ; 5.70g 0. 056mol) in water (sol) was then added and reaction mixture stirred at 5 C for 2 hours, then left to stand at ambient temperature for 24 hours. The mixture was then heated at 80 C for 2.5 hours, allowed to cool and mixture distilled to give the title compound (bp 75-80 C). NMR : 0.2 (q, 2H), 0.14 (q, 2H), 0.96 (s, 3H), 1.42 (s, 2H).

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; ASTRAZENECA AB; ASTRAZENECA UK LIMITED; WO2003/76436; (2003); A1;,
Amide – Wikipedia,
Amide – an overview | ScienceDirect Topics

Synthetic Route of 67341-01-9, 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. 67341-01-9, name is tert-Butyl (2-hydroxy-1-phenylethyl)carbamate belongs to amides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

1-(2,6-difluoro-benzyl)-5-nitro-1H-pyrimidine-2,4-dione (82 mg, 0.29 mmol), ((R)-2-hydroxy-1-phenyl-ethyl)-carbamic acid tert-butyl ester (69 mg, 0.29 mmol), and triphenylphosphine (114 mg, 0.44 mmol) were dissolved in anhydrous tetrahydrofuran (2 mL). To this solution was added diethyl azodicarboxylate (200mu?, 0.44 mmol), followed by stirring at room temperature for 4 hrs. The solution was concentrated, after which the residue was purified using silica gel chromatography (eluent: hexane/ethyl acetate/dichloromethane, 3/1/1) and dried in a vacuum to afford 67 mg of the compound as a colorless oil (yield 67%). 1H NMR (300MHz, CDCl3) delta 1.30(9H, s), 3.40(1H, d), 4.50(1H, m), 5.08-5.27(4H, m), 7.02(2H, t), 7.26-7.47(6H, m), 8.78 (1H, s)

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, tert-Butyl (2-hydroxy-1-phenylethyl)carbamate, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; Sk Chemicals Co., Ltd.; EP2390250; (2011); A2;,
Amide – Wikipedia,
Amide – an overview | ScienceDirect Topics

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. Recommanded Product: 144-80-9

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;,
Amide – Wikipedia,
Amide – an overview | ScienceDirect Topics

Synthetic Route of 24036-52-0,Some common heterocyclic compound, 24036-52-0, name is 6-Bromo-2H-1,4-benzoxazin-3(4H)-one, molecular formula is C8H6BrNO2, 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: Toluene (4.5mL) was added to a flask containing 6-bromo-3,4-dihydroquinolin-2(1H)-one (300mg, 1.33mmol), 3-(trifluoromethoxy)aniline (231muL, 1.73mmol), Pd2(dba)3 (15.2mg, 0.02mmol), 2-dicyclohexylphosphino-2?,4?,6?-triisopropylbiphenyl (31.6mg, 0.07mmol) and NaOt-Bu (192mg, 2.00mmol) under an argon atmosphere. The mixture was stirred at 100C for 9h. After cooling, the reaction mixture was diluted with EtOAc, and filtered through a pad of Celite. The filtrate was concentrated in vacuo. Crude material was purified by flash chromatography with n-hexane/EtOAc (2:3) to afford the desired diaryl amine 11i

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 6-Bromo-2H-1,4-benzoxazin-3(4H)-one, its application will become more common.

Reference:
Article; Takeuchi, Tomoki; Oishi, Shinya; Kaneda, Masato; Misu, Ryosuke; Ohno, Hiroaki; Sawada, Jun-Ichi; Asai, Akira; Nakamura, Shinya; Nakanishi, Isao; Fujii, Nobutaka; Bioorganic and Medicinal Chemistry; vol. 22; 12; (2014); p. 3171 – 3179;,
Amide – Wikipedia,
Amide – an overview | ScienceDirect Topics

Adding a certain compound to certain chemical reactions, such as: 94838-59-2, name is tert-Butyl 4-aminophenethylcarbamate, 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 94838-59-2, Recommanded Product: tert-Butyl 4-aminophenethylcarbamate

Tert-butyl (4-aminophenethyl)carbamate (4.5 g, 21.83 mmol, 1.0 eq) was dissolved in DCM (150 mL) and cooled to 0C using an ice bath. DMAP (1.6 eq) was added in one portion to the stirring mixture followed by dropwise addition of bromoacetyl bromide (1.2 eq) in 50 mL DCM. The mixture was stirred for 30 minutes at 0C and then 1.5 hours at room temperature before it was concentrated in vacuo. The crude material was purified using column chromatography on Si02 with 75-100% EtOAc in heptane as eluent. This gave a colorless solid which was used directly in the next example.

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; UNIVERSITETET I OSLO; GOLDING, Louise; RONGVED, Pal; ASTRAND, Ove Alexander H°gmoen; SAMUELSEN, Ørjan; SCHNAARS, Christian; KILDAHL-ANDERSEN, Geir; (234 pag.)WO2018/33719; (2018); A1;,
Amide – Wikipedia,
Amide – an overview | ScienceDirect Topics

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, Safety of 4-Bromo-N-methylbenzamide

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;,
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. 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. Application In Synthesis of 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;,
Amide – Wikipedia,
Amide – an overview | ScienceDirect Topics

Electric Literature of 7150-72-3, The chemical industry reduces the impact on the environment during synthesis 7150-72-3, name is tert-Butyl vinylcarbamate, I believe this compound will play a more active role in future production and life.

General procedure: A 25 mL round bottom flask or 20 mL glass vial with a stir bar was charged with thiol (1.2 mmol) and enecarbamate or enamide (1.0 mmol) followed by the addition of water (5 mL, 0.2M). The reactions were stirred vigorously at room temperature for 18 hours. The aqueous reaction was extracted with EtOAc (3 x 20 mL). The organic layers were collected and dried with Na2SO4, filtered and the solvent evaporated to provide the crude product. The crude product was purified by column chromatography using hexanes/EtOAc in an increasing polarity up to 1:1 mixture. The fractions containing the desired product were concentrated to provide the desired thioethers.

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, tert-Butyl vinylcarbamate, other downstream synthetic routes, hurry up and to see.

Reference:
Article; Barman, Eliezer; Hourezadeh; Lim, Daniel; Tetrahedron Letters; vol. 60; 34; (2019);,
Amide – Wikipedia,
Amide – an overview | ScienceDirect Topics