Month: January 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. 113100-53-1, name is 1-Methyl-3-(trifluoromethyl)-1H-pyrazole-4-carboxylic acid, A new synthetic method of this compound is introduced below., Product Details of 113100-53-1

General procedure: Intermediate 5 (1.0 mmol) and 4-dimethylaminopyridine (0.1 mmol) were added to a mixture of the corresponding carboxylic acid 6 (1.3 mmol) and (EDCI, 2 mmol) in CH2Cl2 (20 mL). The reaction system was stirred at room temperature overnight and then diluted with CH2Cl2 (50 mL). The resulting mixture was consecutively washed with 10% citric acid solution and brine. Then the organic phase was dried with sodium sulphate and filtered, and concentrated under reduced pressure. The residue was purified on a silica gel column to afford the title compounds 7-17.

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.

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. 180207-57-2, name is 2-(1H-Pyrazol-4-yl)ethanol, This compound has unique chemical properties. The synthetic route is as follows., Formula: C5H8N2O

General procedure: KMnO4 (42.7 g, 0.27 mol) was added in small portions to asolution (in case of compounds 4a-c) or suspension (incase of compound 4d) of alcohol 4 (0.1 mol) and K2CO3 (5 g)in H2O (200 ml) at 70 during 1 h. The mixture washeated with stirring at 80 for 3 h, cooled to room temperature, and the precipitate that formed was filtered off. The mother liquid was acidified by 0.1 M aq HCl topH 5. The precipitated product was filtered and dried atroom temperature in vacuo. 2-Oxo-2-(1H-pyrazol-4-yl)acetic acid (13a). Yield10.6 g (76%). Colorless solid. Mp >280C. 1H NMR spectrum (DMSO-d6), delta, ppm (J, Hz): 8.02 (1H, s, H-5);8.17 (1H, s, H-3). 13C NMR spectrum (DMSO-d6), delta, ppm:119.8 (C-4); 136.5 (C-3); 137.6 (C-5); 164.3 (CO); 185.8(COOH). Mass spectrum (APCI), m/z: 139 [M-H]-. Found, %:C 42.72; H 2.82; N 20.14. C5H4N2O3. Calculated, %:C 42.87; H 2.88; N 20.00.

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 180207-57-2.

Related Products of 37687-24-4, These common heterocyclic compound, 37687-24-4, name is Diethyl 3,5-pyrazoledicarboxylate, 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 10A Diethyl 1-[2-(2,4-dichlorophenyl)-2-oxoethyl]-1H-pyrazole-3,5-dicarboxylate 5 g (23.6 mmol) of diethyl 1H-pyrazole-3,5-dicarboxylate were dissolved in 100 ml of acetone, and 6.3 g (23.6 mmol) of 2-bromo-2,4-dichloroacetophenone and 3.6 g (26 mmol) of potassium carbonate were added. The mixture was stirred at RT for 12 h. The reaction mixture was concentrated and the residue was taken up in water and dichloromethane. The organic phase was washed with saturated aqueous sodium chloride solution, dried over magnesium sulfate and concentrated on a rotary evaporator. The residue was triturated with diethyl ether, and the solid was filtered off with suction. This gave 9.48 g (94% of theory) of the product as a solid. LCMS (method 6): Rt=2.34 min. (m/z=399 (M+H)+) 1H-NMR (400 MHz, DMSO-d6): delta=8.02 (d, 1H), 7.84 (s, 1H), 7.68 (dd, 1H), 7.35 (s, 1H), 6.13 (s, 2H), 4.32 (q, 2H), 4.26 (q, 2H), 1.31 (t, 3H), 1.25 (t, 3H).

The synthetic route of 37687-24-4 has been constantly updated, and we look forward to future research findings.

Reference of 26621-44-3, 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. 26621-44-3, name is 3-Nitro-1H-pyrazole belongs to pyrazoles-derivatives compound, it is a common compound, a new synthetic route is introduced below.

Step 1c Preparation of the Nitropyrazole 4. 3-Nitropyrazole (1.13 g, 10 mmol) in dry DMF (10 ml), under argon, was treated with anhydrous K2CO3 (2.7 g, 15 mmol) and then, dropwise, with methyl-4-bromobutyrate (1.82 g, 10.05 mmol) at RT. After stirring overnight the DMF was removed and the residue partitioned between H2O and EtOAc. The combined organic extracts were washed (H2O and brine), dried (Na2SO4), filtered and evaporated to give a mixture of 4 and 6 (2.05 g) as a pale yellow oil. MS (ES+) m/z 214 (MH+).

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, 3-Nitro-1H-pyrazole, other downstream synthetic routes, hurry up and to see.

Application of 29097-00-5, As we all know, there are many different methods for the synthesis of a compound, and people can choose the synthesis method that suits their own laboratory according to the actual situation. 29097-00-5 name is Methyl 3-amino-1H-pyrazole-4-carboxylate, This compound is widely used in many fields, so it is necessary to find a new synthetic route. The downstream synthesis method of this compound is introduced below.

1.0 g of compound (2′) is added to 10 ml of phosphoric acid to dissolve. This solution is ice-cooled to keep the temperature to -5 to 0C, and 0.54 g of sodium nitrite is added thereto, followed by stirring for 1 hour to obtain a diazonium salt solution. Separately, 20 ml of NMP (N- methylpyrrolidone) is added to 1.60 g of compound (3′) and, under stirring, the aforesaid diazonium salt solution is added thereto at 8C or lower. Simultaneously with completion of the addition, the ice bath is removed, and stirring is continued for further 1 hour. 40 ml of methanol is added to the reaction solution, and the resulting mixture is stirred for 30 minutes. Crystals precipitated are collected by filtration, and spray-washed with 30 ml of methanol. The thus- obtained crystals are added, without drying, to 100 ml of water, followed by stirring at 20 to 25C for 30 minutes. Crystals precipitated are collected by filtration, and sufficiently spray-washed with water. The thus-obtained crystals are added, without drying, to 20 ml of NMP and 10 ml of water, followed by stirring for 30 minutes under heating at 100C. After stirring for 30 minutes at room temperature, crystals precipitated are collected by filtration, and spray-washed with 20 ml of NMP/water=2/l and 20 ml of water. The thus-obtained crystals are dried to obtain 2.0 g of compound D-228 of the invention. Yield: 80%.Infrared absorption chart is shown in Fig. 6.

At the same time, in my other blogs, there are other synthetic methods of this type of compound, Methyl 3-amino-1H-pyrazole-4-carboxylate, and friends who are interested can also refer to it.

Reference of 20154-03-4, A common heterocyclic compound, 20154-03-4, name is 3-(Trifluoromethyl)-1H-pyrazole, molecular formula is C4H3F3N2, 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.

From the indications on page 343 of Ref. refPreviewPlaceHolder49, the following procedure was designed: 3-(trifluoromethyl)-1H-pyrazolerefPreviewPlaceHolder [32] , refPreviewPlaceHolder33 M.E.F. Braibante, G. Clar, M.A.P. Martins and C. Jackson. J. Heterocycl. Chem., 30 (1993), pp. 1159-1160. [33] and refPreviewPlaceHolder[34] (1e) (5.54 g, 40.7 mol) and N-chlorosuccinimide (5.97 g, 44.7 mmol) in acetonitrile (13 mL) were heated in a microwave oven at 120 ¡ãC for 1 h. The resulting mixture was concentrated to dryness and dispersed in water (300 mL). The precipitate was filtered, rinsed with water and left to dry over 3 days to yield compound 3i (5.08 g, 73percent) as a powder; mp 94 ¡ãC 1H NMR (CDCl3): 7.69 (s, 1H); 11.2 (s (br), 1H). 13C NMR (CDCl3): 109.6; 120.2 (q, J=267 Hz); 129.5; 130.0 (q, J=37 Hz). HRMS: calcd for C4H2ClF3N2-H: 168.9780; Found: 168.9747.

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.

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. 3524-32-1, name is 5-Amino-1,3-dimethylpyrazole, This compound has unique chemical properties. The synthetic route is as follows., HPLC of Formula: C5H9N3

The following crystalline form was characterised:2-(2-Chloro-5 -(trifluoromethyl)pyridin-4-ylamino)-6-methoxy-N-methylbenzamide (1.66 g, 4.61 mmol), l,3-dimethylpyrazol-5-amine (0.523 g, 4.71 mmol), palladium(II) acetate (0.083 g, 0.37 mmol), 9,9-dimethyl-4,5-bis(diphenylphosphino)xanthene (0.427 g, 0.74 mmol) and cesium carbonate (1.804 g, 5.54 mmol) were mixed together in dioxane (30 mL). The reaction was degassed with argon and was stirred at 90 0C for 3 hours under argon. The mixture was filtered, the filtrate concentrated and purified twice by flash chromatography on silica gel eluting with 0 to 4% MeOH in DCM/EtOAc (60:40). The solvent was evaporated to dryness to afford 2-(2-( 1,3 -dimethyl- lH-pyrazol-5 -ylamino)-5- (trifluoromethyl)pyridin-4-ylamino)-6-methoxy-N-methylbenzamide (0.882 g, 44.0 %) as a beige solid. 150 mg of this material was dissolved in acetonitrile, concentrated and diluted with DCM. Crystals appeared slowly. The resulting crystalline solid was collected by filtration, washed with DCM and dried to a constant weight to afford 2-[[2-[(2,5- dimethylpyrazol-3-yl)amino]-5-(trifluoromethyl)-4-pyridyl]amino]-6-methoxy-N-methyl- benzamide (110 mg, 32.3 %) as a white crystalline solid. Melting onset of 163C

According to the analysis of related databases, 3524-32-1, the application of this compound in the production field has become more and more popular.

Related Products of 133228-21-4,Some common heterocyclic compound, 133228-21-4, name is N,N-Dimethyl-1H-pyrazole-1-sulfonamide, molecular formula is C5H9N3O2S, 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 stirred solution of S1 (25.3 g, 144 mmol) in THF (200 mL) at -78 C was added dropwise 1.6 M n-butyllithium in hexane (99 ml, 159 mmol). After 30 min, EtI (12.8 mL, 159 mmol) was added dropwise. The reaction mixture was stirred at -78 C for 30 min and allowed to room temperature. After 1 h, the stirring became difficult by formation of white precipitates. THF (200 mL) was added dropwise to give yellow solution. The stirring was continued for 2 h. Then, the mixture was poured into saturated NaHCO3 aq. (600 mL), and extracted with EtOAc (400 mL x2), and the extract was dried over MgSO4, filtered and concentrated under reduced pressure. The residue was purified by column chromatography on silica gel (n-hexane/EtOAc,100:0 to 30:70, v/v) to afford S2 (19.8 g, 68%) as colorless liquid.1H NMR (300 MHz, CDCl3) d 1.30 (3H, t, J = 7.8 Hz), 2.94 (2H, dd, J = 15.0, 7.5 Hz), 3.03 (6H, s), 6.13 (1H, br s), 7.55 (1H, br s).

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route N,N-Dimethyl-1H-pyrazole-1-sulfonamide, its application will become more common.

Related Products of 1015845-73-4, 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 1015845-73-4 as follows.

General procedure: To a fine suspension of 1 mmol of the corresponding amine in 3 ml of anhydrous DMF was added 1 mmol of ethoxycarbonylisothiocyanate. After stirring the mixture for 1 h at room temperature, 30 ml of cold water was added. The precipitated product was filtered, washed with cold water and recrystallized from ethanol.

According to the analysis of related databases, 1015845-73-4, the application of this compound in the production field has become more and more popular.

Electric Literature of 127107-23-7, 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. 127107-23-7, name is 1-Methyl-1H-pyrazol-4-amine hydrochloride, This compound has unique chemical properties. The synthetic route is as follows.

Step 4) fert-butyl 5-((5-chloro-2-((l-methyl-lH-pyrazol-4-yl)amino)pyrimidin-4-yl)amino)-5- (cvanomethyl)hexahydrocvclopentarc1pyrrole-2(lH)-carboxylate [0464] To a suspension of tert-butyl 5-(cyanomethyl)-5-((2,5-dichloropyrimidin-4-yl)amino) hexahydrocyclopenta[c]pyrrole-2(lH)-carboxylate (631.5 mg, 1.53 mmol) and 1-methyl-lH- pyrazol-4-amine hydrochloride (213.2 mg, 1.60 mmol) in -BuOH (10 mL) was added Et3N (322.1 mg, 3.18 mmol). The reaction mixture was stirred at 150 C in a sealed tube overnight and concentrated in vacuo. The residue was purified by silica gel column chromatography (MeOH/DCM (v/v) = 1/50) to give the title compound as a yellow solid (283.0 mg, yield 39.1%). LC-MS (ESI, pos. ion) m/z: 473.3 [M+H]+.

The chemical industry reduces the impact on the environment during synthesis 1-Methyl-1H-pyrazol-4-amine hydrochloride. I believe this compound will play a more active role in future production and life.