Day: February 4, 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. 121507-34-4, name is 5-Isopropoxy-1H-pyrazol-3-amine, A new synthetic method of this compound is introduced below., Application In Synthesis of 5-Isopropoxy-1H-pyrazol-3-amine

5-bromo-N’-(5-isopropoxy-1H-pyrazol-3-yl)-N-[(3-methylisoxazol-5-yl)methyl]pyrimidine-2,4-diamine (also known as 5-bromo-N-[(3-methyl-1,2-oxazol-5-yl)methyl]-N’-(5-propan-2-yloxy-1H-pyrazol-3-yl)pyrimidine-2,4-diamine), used as starting material, was prepared as follows: a) To a solution of 5-isopropoxy-1H-pyrazol-3-amine (2.0 g, 14.2 mmol) in dry tetrahydrofuran (60 ml) under a nitrogen atmosphere was added triethylamine and the mixture cooled to 0 C. A solution of 5-bromo-2,4-dichloropyrimidine (3.23 g, 14.2 mmol) in dry tetrahydrofuran (30 ml) was added dropwise and the mixture was allowed to stir at room temperature for 18 hours. The mixture was evaporated and the residue crystallised with ethyl acetate. The mixture was filtered and the residue triturated thoroughly with water. The resultant solid was filtered and then left to dry overnight to give 5-bromo-2-chloro-N-(5-isopropoxy-1H-pyrazol-3-yl)pyrimidin-4-amine (1.645 g, 35% yield). MS: m/z 332 (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.

Some common heterocyclic compound, 17635-45-9, name is 4-Pyrazol-1-yl-phenylamine, molecular formula is C9H9N3, 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-Pyrazol-1-yl-phenylamine

[0183] A mixture of intermediate 33 (0.10 g, 0.28 mmol) and 4-pyrazol-l-yl-phenylamine (50 mg, 0.31 mmol) in acetic acid (3 mL) was sealed in a microwave reaction tube and irradiated with microwave at 130 ¡ãC for 15 min. After cooling to room temperature, the cap was removed and the mixture concentrated. The residue was taken up in water (20 mL) and neutralized with 10percent NaOH solution until solid precipitated. The brown solid was filtered and then purified by HPLC. The corrected fractions were combined and poured into saturated NaHCO3 solution (30 mL). The combined aqueous layers were extracted with EtOAc (2 x 30 mL) and the combined organic layers washed with brine, dried over anhydrous Na2SO4 and filtered. The filtrate was concentrated and the resulting solid dissolved in minimum amount of EtOAc and hexanes added until solid precipitated. After filtration, the title compound was obtained as a white solid (15 mg, 11percent).[0184] 1H NMR (500 MHz, DMSO-d6): delta 1.12 (s, 9H), 2.15 (s, 3H), 6.49 (t, J= 2.2 Hz, IH), 7.50-7.55 (m, 2H), 7.58 (s, IH), 7.62 (d, J= 9.1 Hz, 2H), 7.68 (d, J= 1.3 Hz, IH), 7.77 (d, J= 9.1 Hz, 2H), 7.96 (s, IH), 8.11 (s, IH), 8.13-8.16 (m, IH), 8.33 (d, J= 2.5 Hz, IH), 8.64 (s, IH), 9.17 (s, IH). MS (ES+): m/z 478 (M+H)+.

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 17635-45-9, its application will become more common.

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. 1280210-79-8, name is tert-Butyl 4,6-dihydropyrrolo[3,4-c]pyrazole-5(2H)-carboxylate, This compound has unique chemical properties. The synthetic route is as follows., HPLC of Formula: C10H15N3O2

Synthesis of 257-A and 258-A. A mixture of tert-butyl 4,6-dihydropyrrolo[3,4- c]pyrazole-5(2H)-carboxylate (314 mg, 1.50 mmol), Cs2CO3 (978 mg, 3.00 mmol) and iodomethane (320 mg, 2.25 mmol) in DMF (6 mL) was stirred at room temperature for 16 h. The mixture was diluted with water (18 mL), extracted with EtOAc (10 mL ¡Á 3). The combined organic layer was washed with brine (10 mL ¡Á 3), dried over anhydrous Na2SO4 and then concentrated in vacuo. The residue was purified by column chromatography on silica gel (DCM : MeOH = 100 : 1 ~ 50 : 1) to give 257-A and 258-A (270 mg, 81%) as a yellow solid.

According to the analysis of related databases, 1280210-79-8, the application of this compound in the production field has become more and more popular.

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. 146941-72-2, name is 4-Bromo-1-methyl-1H-pyrazol-3-amine, A new synthetic method of this compound is introduced below., Quality Control of 4-Bromo-1-methyl-1H-pyrazol-3-amine

A) Methyl 3-(4-bromo-1-methyl-1H-pyrazol-3-ylamino)propanoate A mixture of 4-bromo-1-methyl-1H-pyrazol-3-amine (3.50 g), methyl acrylate (8 mL), 4-(dimethylamino)pyridine (0.49 g) and DMF (3 mL) was stirred at 135C for 3 hours and 30 minutes under irradiation with microwave. Water and ethyl acetate were added to the reaction mixture to separate an organic layer. The aqueous layer was subjected to extraction with ethyl acetate. The combined extract was washed with saturated brine and dried over anhydrous sodium sulfate, and the solvent was distilled off under reduced pressure. The residue was purified by silica gel column chromatography (ethyl acetate/petroleum ether) to obtain the title compound (3.20 g). MS: [M+H]+ 261.8.

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 1355249-29-4, These common heterocyclic compound, 1355249-29-4, name is Ethyl 4-iodo-1-(4-methoxybenzyl)-1H-pyrazole-3-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.

Step A: ethyl 1-(4-methoxybenzyl)-4-(7-{[2-(trimethylsilyl)ethoxy]methyl}-7H-pyrrolo[2,3-d]pyrimidin-4-yl)-1H-pyrazol-3-formate Under the protection of nitrogen gas, to a solution of ethyl 4-iodo-1-(4-methoxybenzyl)-1H-pyrazol-3-formate (1.0 g, 2.6 mmol, 1.0 eq., prepared from the step C of Example 26), diboronic acid pinacol ester (0.7 g, 2.8 mmol, 1.1 eq.) and potassium acetate (0.76 g, 7.8 mmol, 3.0 eq.) in DMSO (30 mL) was added Pd(dppf)Cl2 (95 mg, 0.13 mmol, 0.05 eq.). The reactants were protected with nitrogen gas and stirred overnight at 80C. After the resulting mixture was cooled to room temperature, the resulting mixture was diluted with water and ethyl acetate, and extracted with ethyl acetate. The combined organic phase was washed with water and brine, dried over sodium sulfate, filtered and concentrated in vacuo to give 3-(ethoxycarbonyl)-1-(4-methoxybenzyl)-1H-pyrazol-4-yl boronic acid pinacol ester (1.2 g) as a crude product.

The synthetic route of 1355249-29-4 has been constantly updated, and we look forward to future research findings.

Synthetic Route of 70951-85-8,Some common heterocyclic compound, 70951-85-8, name is 4-Bromo-1-(tert-butyl)-1H-pyrazole, molecular formula is C7H11BrN2, 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.

Synthesis of 1 -tert-Butyl-4-(4,4,5,5-tetramethyl-1 ,3,2-dioxaborolan-2-yl)pyrazole 4.19To a stirred mixture of 50 g of 4-bromo-1 -tert-butyl-pyrazole 3J. in 230 mL THF was added dropwise 100 mL 2.5M N-butyllithium solution in hexane under argon atmosphere below – 60 C, then the mixture was stirred at this temperature for 5 min, before 52 mL 2-isopropoxy- 4,4,5,5-tetramethyl-1 ,3,2-dioxaborolane were added dropwise below -60 C. The reaction mixture was allowed to reach ambient temperature. The mixture was cooled with an ice bath and diluted with aqueous phosphate buffer solution and water and neutralized with 2M aqueous hydrochloric acid. The organic solvent was removed by destination and the residue was extracted with DCM. The combined organic extracts were washed with saturated brine, dried over sodium sulfate, filtered and concentrated in vacuo to yield 44.26 g of 1 -tert-butyl-4- (4,4,5,5-tetramethyl-1 ,3,2-dioxaborolan-2-yl)pyrazole as solid.Analysis: HPLC-MS: Rt = 0.904 min (method F), M+H = 251

The synthetic route of 70951-85-8 has been constantly updated, and we look forward to future research findings.

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. 3112-31-0, name is 1H-Pyrazole-3,5-dicarboxylic acid, This compound has unique chemical properties. The synthetic route is as follows., Recommanded Product: 3112-31-0

Example 4-15: Synthesis of 5-[(R)-1-(3”Chloro-biphenyl-4-ylmethyl)-2~ethoxycarbonyl- ethylcarbamoyO-1 H-pyrazole-3-carboxyUc acid; To a mixture of Intermediate 17-1 (130 mg, 0.367 mmol), 1H-pyrazole-3,5-dicarboxylic acid (74.5 mg, 0.477 mmol), EDCI (91 mg, 0.477 mmol) and HOBt (64.5 mg, 0.477 mmof) in DMF (3 ml) is added triethylamine (149 mg, 0.203 mmol) and the mixture is stirred at room temperature for 18 hours. Any insoluble material is removed by filtration and the filtrate is chromatographed by HPLC using a gradient of 10percent MeCN/water to 100percent MeCN (+0.1percent TFA). Lyophitization of the proper fractions gives the title compound; HPLC Retention time 1.31 minutes (condition C); MS 456.2 (M+1); 1H NMR (400 MHz, DMSO-d6) delta ppm 1.12 (t, J=7,07 Hz1 3H), 2.54-2.67 (m, 2H)1 2.84-2.97 (m, 2H), 4.02 (q. J=7.07 Hz, 2H), 4.54 (m, 1H)1 7.11 (s, broad, 1H), 7.32 (d, J=8.08 Hzt 2H), 7.39 (m, 1H), 7.46 (t, 1 H)1 7.62 (d, J=8.08 Hz, 3H)1 7.69 (s. 1H), 8.41 (s, broad, 1H).

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 3112-31-0.

These common heterocyclic compound, 26621-44-3, name is 3-Nitro-1H-pyrazole, 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. Computed Properties of C3H3N3O2

A solution of 3-nitro-1H-pyrazole (Intermediate 2, 250 mg, 2.21 mmol) was dissolved in anhydrous N,N-dimethylformamide (5 mL) was treated with a 60% dispersion of sodium hydride in mineral oil (93 mg, 2.32 mmol) was added while stirring under nitrogen. After the effervescence ceased, the reaction stirred for an additional 10 min. At this time, the reaction was treated with (2-bromo-ethoxy)-tert-butyl-dimethyl-silane (598 mg, 2.50 mmol). The reaction continued to stir under nitrogen for 2 h. At this time, the solution was diluted with ethyl acetate (200 mL), washed with water (2¡Á75 mL), a saturated aqueous sodium chloride solution (75 mL), dried over magnesium sulfate, filtered and concentrated in vacuo. Silica gel column chromatography (Merck silica gel 60, 40-63 mum; 5-25% ethyl acetate/hexanes) afforded 1-[2-(tert-butyl-dimethyl-silanyloxy)-ethyl]-3-nitro-1H-pyrazole (508 mg, 84%) as a yellow oil. 1H-NMR (400 MHz, DMSO-d6) delta 0.00 (6H, s), 0.86 (9H, s), 4.03 (2H, t, J=5.6 Hz), 4.40 (2H, t, J=5.2 Hz), 7.11 (1H, d, J=2.4 Hz), 8.06 (1H, d, J=2.4 Hz).

The synthetic route of 3-Nitro-1H-pyrazole 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. 162758-35-2, name is 5-(4-Chlorophenyl)-1-(2,4-dichlorophenyl)-4-methylpyrazole-3-carboxylic acid, A new synthetic method of this compound is introduced below., SDS of cas: 162758-35-2

General procedure: To a mixture of carboxylic acid (1 mmol), EDC¡¤HCl (1.2 mmol) and HOBt (1.2 mmol) in dry dichloromethane (10 mL) was added a mixture of amine (1 mmol) and triethyl amine (1.5 mmol) in dichloromethane (5 mL) at 0 C. The mixture was stirred at room temperature till the completion of reaction (judged by TLC). The reaction mixture was diluted with additional DCM (20 mL). The organic layer was washed with water, brine and dried (Na2SO4). Concentration and purification over silica gel (100-200 mesh) afforded the desired compound.

The synthetic route of 162758-35-2 has been constantly updated, and we look forward to future research findings.

Synthetic Route of 16461-94-2, 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. 16461-94-2, name is 4-Bromo-1H-pyrazol-3-amine belongs to pyrazoles-derivatives compound, it is a common compound, a new synthetic route is introduced below.

3-Amino-4-bromopyrazole (5 g, 30.9 mmol) and 4-methoxybenzyl chloride (21 g, 134 mmol, 4.3 equiv.) werecombined in anhydrous DMF (25 mL) and added dropwise to a stirred suspension of sodium hydride (60% dispersionin mineral oil, 6.25 g, 156 mmol, 5 equiv.) in anhydrous DMF (50 mL). The presuming suspension was stirred 2 days atroom temperature. Water (300 mL) was added slowly and the resulting mixture was extracted with ether (4 x 350 mL).The organic layers were combined, washed with brine, dried over anhydrous sodium sulfate and concentrated underreduced pressure. The crude product was dissolved in dichloromethane and purified by silica gel chromatography using a gradient from 10% to 20% ethyl acetate-hexanes. The product, a white solid, is obtained as a 60:40 mixture of the 1-benzylated-1 H product and the 2-benzylated-2H product (14.96 g total, 93% yield).

The synthetic route of 4-Bromo-1H-pyrazol-3-amine has been constantly updated, and we look forward to future research findings.