Author: tianli

14433-76-2, 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. 14433-76-2, name is N,N-Dimethylcapramide belongs to amides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

the reaction formula of this embodiment is as follows:In a 25 ml reaction flask, add compound 1a (0.3mmol, 0.1561g), compound 2j (3mmol, 0.5980g), water 1.5 muL), toluene (1.5mL) to dissolve the above materials, and stir the reaction at 80 C. The reaction time is 3h After the reaction was completed, the solvent was removed by spin-drying, and the residue was subjected to flash column chromatography (PE: EA = 30: 1) to obtain pure 3aj (0.0850 g) with a yield of 85%.

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

Reference:
Patent; Xuzhou Medical University; Wu Nan; Xu Zhou; Mi Jiajia; Li Chuang; Yuan Changyong; Zheng Yan; (15 pag.)CN110668937; (2020); A;,
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 402-46-0 as follows. 402-46-0

A round bottom flask was charged with 4-fluorobenzenesulfonamide (945 mg, 5.4 mmol), L-proline-t-butyl ester HCl (1.24 g, 6 mmol), and cesium carbonate (4.2 g, 12 mmol) and suspended in 10 ml anhydrous DMSO. The mixture was placed in a preheated oil bath and equipped with a condenser, and heated under nitrogen at 168 oC overnight. HPLC analysis of the mixture indicated complete conversion of the benzenesulfonamide starting material. The mixture was transferred to an Erlenmeyer flask, the reaction pot was diluted with 2 ml of concentrated HCl, and added to the mixture in the Erlenmeyer flask and allowed to stir. The aqueous was then extracted with ethyl acetate (3 x 50 ml), and the combined extracts were washed with water (3 x 15 ml). The volatiles were then removed under vacuum, and 1.24 g of crude material was obtained. The desired intermediate was isolated using MPLC, utilizing a 0 to 60% gradient of acetone in DCM, affording 0.56 g (41%):1H NMR (300 MHz, DMSO-d6)d ppm 7.58 (d, J= 9.0 Hz, 2H), 6.98 (s, 2H), 6.54 (d, J= 9.0 Hz, 2H), 4.28 (d, J= 8.4 Hz, 1H), 2.35-2.22 (m, 2H), 2.04-1.96 (m, 2H).

According to the analysis of related databases, 402-46-0, the application of this compound in the production field has become more and more popular.

Reference:
Article; Ahmed, Gulzar; Elger, Walter; Meece, Frederick; Nair, Hareesh B.; Schneider, Birgitt; Wyrwa, Ralf; Nickisch, Klaus; Bioorganic and Medicinal Chemistry; vol. 25; 20; (2017); p. 5569 – 5575;,
Amide – Wikipedia,
Amide – an overview | ScienceDirect Topics

92136-39-5, 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. 92136-39-5, name is N-Boc-Propargylamine, A new synthetic method of this compound is introduced below.

EXAMPLE 314A tert-butyl allylcarbamate A solution of copper cyanide (1.15 g, 12.9 mmol) in THF (30 mL) at -78 C. was treated slowly with n-butyllithium (16.9 mL, 27.1 mmol), stirred for 15 minutes at -78 C., treated with tributyltin hydride (7.88 g, 7.30 mL, 27.1 mmol) over a period of 5 minutes, stirred for 15 minutes, treated with tert-butyl 2-propynylcarbamate (2.00 g, 12.9 mmol) in tetrahydrofuran (7 mL), stirred at -78 C. for 1 hour, and treated with a 9:1 aqueous solution of ammonium chloride:ammonium hydroxide (250 mL) and dichloromethane (200 mL). The suspension was filtered through a short pad of diatomaceous earth (Celite). The organic phase of the filtrate was washed with brine and concentrated. The residue was purified on silica gel using 1-2% ethyl acetate/heptane to provide the desired product (3.66 g, 63%). 1H NMR (400 MHz, CDCl3) delta 6.08 (dt, B part of an AB system, J=19.3 Hz, 1.3 Hz, 1H); 5.93 (dt, A part of an AB system, J=19.3 Hz, 4.8 Hz, 1H), 4.59 (br s, 1H), 3.78 (br s, 2H), 1.45 (s, 9H), 1.32-1.26, (m, 12H), 0.90-0.85 (m, 15H).

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; Betschmann, Patrick; Burchat, Andrew F.; Calderwood, David J.; Curtin, Michael L.; Davidsen, Steven K.; Davis, Heather M.; Frey, Robin R.; Heyman, Howard R.; Hirst, Gavin C.; Hrnciar, Peter; Michaelides, Michael R.; Muckey, Melanie A.; Rafferty, Paul; Wada, Carol K.; US2005/26944; (2005); A1;,
Amide – Wikipedia,
Amide – an overview | ScienceDirect Topics

These common heterocyclic compound, 112-84-5, name is Erucamide, 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. 112-84-5

To a solution of LAH (2.30 g, 29.6 mmol) in dry THF (100 mL) was added a solution ofcis-docosenoamide (6) (10.0 g, 29.7 mmol) in dry THF (100 mL) and refluxed. After 12 hthe reaction mixture was cooled and Na2SO4¡¤10H2O was added slowly until the reactionceased. The solution was filtered and concentrated in vacuo to affordcis-docos-13-enylamine (9) (9.55 g, 29.6 mmol, quant.) as a pale yellow oil.

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 112-84-5.

Reference:
Article; Reimann, Marcel; Sandjo, Louis P.; Antelo, Luis; Thines, Eckhard; Siepe, Isabella; Opatz, Till; Beilstein Journal of Organic Chemistry; vol. 13; (2017); p. 1430 – 1438;,
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 6973-09-7 as follows. 6973-09-7

To a solution of Intermediate Example 4 (200 mg, 0.695 mmol) and 5-amino-2- methylbenzenesulfonamide (129.4 mg, 0.695 mmol) in isopropanol (6 ml) was added 4 drops of cone. HCI. The mixture was heated to reflux overnight. The mixture was cooled to rt and diluted with ether (6 ml). Precipitate was collected via filtration and washed with ether. The hydrochloride salt of 5-({4-[(2,3-dimethyl-2H-indazol~6- yl)(methyl)amino]-pyrimidin-2-yl}amino)-2-methylbenzenesulfonamide was isolated as an off-white solid. 1H NMR (400 MHz, d6DMSO+NaHCO3) delta 9.50 (br s, 1 H), 8.55 (br s, 1 H), 7.81 (d, J= 6.2 Hz, 1 H), 7.75 (d, J = 8.7 Hz1 1 H), 7.69 (m, 1 H), 7.43 (s, 1 H), 7.23 (S1 2H), 7.15 (d, J= 8.4 Hz1 1H), 6.86 (m, 1 H), 5.74 (d, J= 6.1 Hz, 1 H), 4.04 (s, 3H), 3.48 (S1 3H)1 2.61 (s, 3H)1 2.48 (s, 3H). MS (ES+, m/z) 438 (M+H).

According to the analysis of related databases, 6973-09-7, the application of this compound in the production field has become more and more popular.

Reference:
Patent; SMITHKLINE BEECHAM CORPORATION; WO2007/64753; (2007); A2;,
Amide – Wikipedia,
Amide – an overview | ScienceDirect Topics

A common compound: 3984-14-3, name is N,N-Dimethylsulfamide, belongs to amides-buliding-blocks compound, it can change the direction of chemical reaction, and react with certain compounds to generate new functional products. A new synthetic method of this compound is introduced below. 3984-14-3

lH-pyrazole-4-carboxylic acid, 5-[13-cyclohexyl-10- [[[(dimethylamino)sulfonyl] amino] carbonyl]-3-methoxy-7H-indolo[2,l- a][2]benzazepin-6-yl]-l,3-dimethyl-, methyl ester.; To a solution of 7H-indolo[2,l-alpha][2]benzazepine-10-carboxylic acid, 13- cyclohexyl-S-methoxy–^-^ethoxycarbony^-l^-dimethyl-lH-pyrazol-S-yl]- (120 mg, 0.222 mmol) in TetaF (5 mL), CDI (54.1 mg, 0.334 mmol) was added. The reaction mixture was heated at 6O0C for one hour, and then allowed to cool to room temperature. N,N-dimethylsulfamide (83 mg, 0.667 mmol) and DBU (0.067 mL,0.445 mmol) were then added and the resultant mixture was heated at 6O0C overnight. The reaction was then quenched with IN HCl solution and the product extracted with ethyl acetate (2 x 3OmL). The organic layers were combined, washed with IN HCl solution, brine, dried (MgSC^) and then filtered. Evaporation of solvents gave the curde product as an orange colored thick oil. This material was then purified by preparative etaPLC using Ceta3CN-eta2O-TFA as a solvent system.Homogeneous fractions were combined and concentrated under vacuum to provide the title compound as an orange colored solid, (31.4 mg, 0.049 mmol, 21.87 % yield). MS m/z 646(MH+), Retention time: 2.245min. (basic). IH NMR (500 MHz, CHLOROFORM-D) delta ppm 1.18 – 1.60 (m, 4 H) 1.70 – 2.14 (m, 6 H) 2.49 (s, 3 H) 2.80 – 2.91 (m, 1 H) 3.05 (s, 6 H) 3.24 (s, 3 H) 3.68 (s, br, 3 H) 3.91 (s, 3 H) 4.64 -4.74 (m, br, 1 H) 4.86 – 5.00 (m, br, 1 H) 6.74 (s, 1 H) 6.94 (d, J=2.75 Hz, 1 H) 7.08 (dd, J=8.85, 2.75 Hz, 1 H) 7.35 (dd, J=8.55, 1.53 Hz, 1 H) 7.53 (d, J=8.55 Hz, 1 H)7.75 (d, J=1.22 Hz, 1 H) 7.89 (d, J=8.54 Hz, 1 H) 8.44 (s, 1 H).

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, 3984-14-3, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; BRISTOL-MYERS SQUIBB COMPANY; WO2009/29384; (2009); A2;,
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. 830-43-3, name is 4-(Trifluoromethyl)benzenesulfonamide, This compound has unique chemical properties. The synthetic route is as follows., 830-43-3

Combine p-trifluoromethylbenzenesulfonamide (112.6 mg, 0.5 mmol), iridium catalyst (5.1 mg, 0.005 mmol, 1 mol%), potassium hydroxide (28 mg, 0.5 mmol, 1 equiv), and methanol (0.3 mL), water (0.9 mL) was sequentially added to the reaction vessel. After the reaction mixture was reacted at 130 C for 12 hours in a reaction vessel, it was cooled to room temperature. The solvent was removed by rotary evaporation, and then the purified target compound was obtained by column chromatography (developing solvent: petroleum ether / ethyl acetate), yield: 90%.

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 of Science and Technology; Meng Chong; Tang Yawen; Li Feng; (10 pag.)CN110857278; (2020); A;,
Amide – Wikipedia,
Amide – an overview | ScienceDirect Topics

1103234-56-5, The chemical industry reduces the impact on the environment during synthesis 1103234-56-5, name is 2,6-Difluoro-3-(propylsulfonamido)benzoic acid, I believe this compound will play a more active role in future production and life.

2,6-Difluoro-3-(propylsulfonamido)benzoic acid (20.O g, 71.6 mmol) was dissolved in acetone (400 mL), and potassium carbonate (29.7 g, 215 mmol) was added. After stirring for 5 minutes, methyl iodide (13.4 mL, 215 mmol) was added. The reaction mixture was stirred overnight. The reaction mixture was filtered and the filtrate concentrated. The crude product was partitioned between ethyl acetate and water and the organic layer washed by brine, dried over MgSO4 and concentrated to dryness. Further removal of solvent under high vacuum afforded methyl 2,6-difluoro-3-(N-methylpropylsulfonamido)benzoate as light yellow solid (17.0 g, 77% yield). 1H NMR (500 MHz, CDCl3) delta 7.57 (td, IH), 7.10 – 6.89 (m, IH), 3.96 (s, 3H), 3.31 (s, 3H), 3.13 – 2.96 (m, 2H), 2.01 – 1.81 (m, 2H), 1.07 (t, 3H).

The chemical industry reduces the impact on the environment during synthesis 2,6-Difluoro-3-(propylsulfonamido)benzoic acid. I believe this compound will play a more active role in future production and life.

Reference:
Patent; ARRAY BIOPHARMA INC.; GENENTECH, INC.; ALIAGAS, Ignacio; GRADL, Stefan; GUNZNER, Janet; MATHIEU, Simon; RUDOLPH, Joachim; WEN, Zhaoyang; WENGLOWSKY, Steven Mark; WO2011/25947; (2011); A1;,
Amide – Wikipedia,
Amide – an overview | ScienceDirect Topics

177906-48-8, The chemical industry reduces the impact on the environment during synthesis 177906-48-8, name is trans-N-Boc-1,4-cyclohexanediamine, I believe this compound will play a more active role in future production and life.

[0311] To a stirred solution of 5-cyclopropyl-4-iodoisoxazole-3-carboxylic acid (1.0 g, 3.59 mmol) in DMF (10 ml) was added EDCI (0.892 g, 4.66 mmol) and HOBT (0.533 g, 3.94 mmol). The solution was stirred for 10 min at 0 C. Next tert-butyl ((lr,4r)-4- aminocyclohexyl)carbamate (0.769 g, 3.59 mmol) was added and the reaction was stirred at rt for 2hr. The progress of the reaction was monitored by TLC. After complete consumption of starting material, the reaction was quenched with water and the solid precipitated was collected by filtration and dried under reduced pressure to obtain a residue. The material was purified by column chromatography to afford tert-butyl ((lr,4r)-4-(5-cyclopropyl-4-iodoisoxazole-3-carboxamido)cyclohexyl)carbamate (0.48 g, 28 %).

The chemical industry reduces the impact on the environment during synthesis trans-N-Boc-1,4-cyclohexanediamine. I believe this compound will play a more active role in future production and life.

Reference:
Patent; EPIZYME, INC.; FOLEY, Megan Alene Cloonan; KUNTZ, Kevin Wayne; MILLS, James Edward John; MITCHELL, Lorna Helen; MUNCHHOF, Michael John; HARVEY, Darren Martin; (208 pag.)WO2016/40498; (2016); A1;,
Amide – Wikipedia,
Amide – an overview | ScienceDirect Topics

2886-65-9, 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. 2886-65-9, name is 7-Chloro-5-(2-fluorophenyl)-1H-benzo[e][1,4]diazepin-2(3H)-one, This compound has unique chemical properties. The synthetic route is as follows.

EXAMPLE 1 7-Chloro-5-(2-fluorophenyl)-2-methylamino-3H-1,4-benzodiazepine A solution of 200 g. (0.695 m) of 7-chloro-1,3-dihydro-5-(2-fluorophenyl)-2H-1,4-benzodiazepin-2-one in 2 l. of tetrahydrofuran and 250 ml. of benzene was saturated with methylamine with cooling in an ice bath. A solution of 190 g. (1 m) of titaniumtetrachloride in 250 ml. of benzene was added through a dropping funnel within 15 minutes. After addition the mixture was stirred and refluxed for 3 hours. Water, 600 ml., was added slowly to the cooled reaction mixture. The inorganic material was separated by filtration and was washed well with tetrahydrofuran. The water layer was separated and the organic phase was dried over sodiumsulfate and evaporated. The crystalline residue was collected with m.p. 204-206. The analytical sample was recrystallized from methylene chloride/ethanol, m.p. 204-206.

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; Hoffmann-La Roche Inc.; US4280957; (1981); A;,
Amide – Wikipedia,
Amide – an overview | ScienceDirect Topics