Month: February 2021

Reference of 52222-73-8,Some common heterocyclic compound, 52222-73-8, name is 4-(Trifluoromethyl)-1H-pyrazole, molecular formula is C4H3F3N2, 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.

For the synthesis of the intermediates 1-3.2.1 17 and 1-3.2.118 to the educt 1-3.1.2 with the appropriate amine in MeOH 0.14 eq copper(I)oxide is added (as shown in Table 15).

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

Adding a certain compound to certain chemical reactions, such as: 174891-10-2, name is 5-Amino-1H-pyrazole-3-acetic acid, belongs to pyrazoles-derivatives 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 174891-10-2, Quality Control of 5-Amino-1H-pyrazole-3-acetic acid

Compound 7 (96 g, 0.395 mol, 1.0 eq.) and compound 4 (83.5 g, 0.592 mol, 1.5 eq.) were suspended in 960 mL of AcOH at 18-2O0C. The suspension was heated to 100- 1020C, and stirred for 2.5 h at this temperature. The suspension was cooled down to 18-2O0C, and filtered. Filtrate cake was washed with 50 mL of AcOH, followed by 100 mL of EtOAc. Solid was collected and dried under vacuum at 5O0C (12 h) to give 136 g of compound 10 with 96.5% HPLC purity in 98.9% yield.

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, 5-Amino-1H-pyrazole-3-acetic acid, other downstream synthetic routes, hurry up and to see.

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. 16034-46-1, name is 1-Methyl-1H-pyrazole-5-carboxylic acid, A new synthetic method of this compound is introduced below., Formula: C5H6N2O2

Example 29 To a 50 ml_ flask containing 20 ml_ of DMF was added 1 mL of oxalyi chloride siowly and stirred for 10 min at RT. 100 mg of 2-Methyi-2H-pyrazole-3-carboxyiic acid was dissolved in 2 mL of the above solution and stirred for 5 min at RT. Then 50 mg of E was dissolved in 1 mL pyridine and added to the above solution. The reaction was completed in 5 min at RT and quenched with 1 mL NH4OH. The solvent was then evaporated under vacuum and the residue dissolved in CH3CN and water and purified with prep HPLC (0% to 95% water/ Acetonitriie) to afford 29 (29mg, 46%).1H-NMR (DMSO, 300 MHz): delta 10.23 (s, 1 H), 8.54 (d, J = 3.9 Hz, 1 H), 7.77 (d, J = 6.9 Hz, 1 H)1 7.66 (s, 1 H), 7.52 (d, J = 7.8 Hz, 2H)1 7.26 (t, J = 6.6 Hz, 1 H), 7.08 (t, J = 7.8 Hz, 1 H), 6.99-6.91 (m, 3H), 6.82 (d, J = 1.2 Hz, 1 H), 4.87 (me, 1 H), 4.03 (s, 3H), 3.22-3.10 (m, 3H)1 2.83-2.80 (m, 1 H), 0.70 (m, 2H), 0.56 (m, 2H).LCMS m/z [M+Hf C28H25N5O3S requires: 512.59. Found 512.12HPLC Tr (min), purity %: 2.95, 98%

The synthetic route of 16034-46-1 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. 4522-35-4, name is 3-Iodo-1H-pyrazole, A new synthetic method of this compound is introduced below., Recommanded Product: 3-Iodo-1H-pyrazole

A solution of 3-iodo-lH-pyrazole (500 mg, 2.6 mmol) and ethylene carbonate (238 mg, 2.70 mmol) was formed in DMF (5 mL) and heated at 150C for 3 h. The mixture was allowed to cool then evaporated under vacuum to remove the solvent. Purification of the residue by FCC eluting with a gradient of 0-100% EtOAc in cyclohexane gave crude title compound (444 mg, 72%) as a brown oil. LCMS (Method 3): Rt 2.17 min, m/z 239 [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.

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. 863548-52-1, name is (1-Methyl-1H-pyrazol-5-yl)methanamine, A new synthetic method of this compound is introduced below., SDS of cas: 863548-52-1

General procedure: To a solutionof the corresponding aldehyde (1.2 eq.; unless stated otherwise) in DMF (2 inL per 0.3 mmol of aldehyde; unless stated otherwise) was added the corresponding amine (2.5 eq.; unless stated otherwise) and the resulting solution was stirred at 25 C to form the corresponding inline. Then, the corresponding isocyano(tosyl)methyl)arene reagent (1 eq.; unless stated otherwise) and K2CO3 (1.5 eq.; unless stated otherwise*) were added and the reaction mixture was stirred at 25 C (unless stated otherwise). The reaction was stopped after the time indicated for each particular reaction. The reaction progress was monitored by TLC. (0083) A saturated aqueous solution of NH4CI (10 mL per 1 mmol of aldehyde) was added to the reaction mixture, which was then extracted with EtOAc (2 x 30 mL per 1 mmol of aldehyde). The combined organic extracts were washed with H2O (2 x 25 mL per 1 mmol of aldehyde), dried over MgSCC, filtered, and the solvent was evaporated in vacuo to provide the crude product. The residue obtained after the workup was purified using column chromatography or preparative TLC (unless stated otherwise). (0084) * note: in cases when the amine was used as HC1 salt, 4 eq. of K2CO3 were used

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 176969-34-9, 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. 176969-34-9 name is 3-(Difluoromethyl)-1-methyl-1H-pyrazole-4-carboxylic acid, 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.

The main procedure is shown in Scheme 2. The raw products of compound 7 were synthesized via one-pot method in a flask containing compounds 5 (30 mmol), 6 (30 mmol), K2CO3 (15 mmol) and PEG1000 (0.45 mmol). The reactions were carried out under stirring at 185 C and were monitored by TLC. After reactions completion, the desired diphenylamine derivatives 7 were obtained via column chromatographic purification. Next, compounds 7 (20 mmol), reductive iron powder (60 mmol), solid NH4Cl (60 mmol) and ethanol aqueous solution (75%, 50 mL) were added. The reactions proceeded with refluxing for 3 h at 90 C and compounds 8 were obtained. Then, compound 3 (30 mmol) and SOCl2 (thionylchloride, 30 mL) were added. The mixture was heated to reflux at 90 C for 3 h. Residual SOCl2 was removed by vacuum distillation in order to obtain compound 4. Finally, the primary amines 8 (10 mmol) dissolved in dichloromethane (CH2Cl2, 5 mL) and triethylamine(Et3N, 10 mL) were added. The mixture was cooled to 0 C and compound 4 (20 mmol) dissolved in dichloromethane (CH2Cl2, 10 mL) was added dropwise under stirring at a temperature not exceeding 5 C. The final mixture was stirred at room temperature for 10 h and the target compounds 9a, 9b and 9c were purified via column chromatography and recrystallization.

At the same time, in my other blogs, there are other synthetic methods of this type of compound, 3-(Difluoromethyl)-1-methyl-1H-pyrazole-4-carboxylic acid, and friends who are interested can also refer to it.

Some common heterocyclic compound, 5334-40-7, name is 4-Nitro-1H-pyrazole-3-carboxylic acid, molecular formula is C4H3N3O4, 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. Formula: C4H3N3O4

4-Nitropyrazoie-3-carboxylic acid (10 g; 63.66 mmol) was added to a stirred solution of 4-fluoroaniline (6.7 ml; 70 mmol), EDC (14.6 g; 76.4 mmol), and HOBt (10.3 g; 76.4 mmol) in DMF (25 ml), then stirred at room temperature overnight. The solvent was removed by evaporation under reduced pressure and the residue triturated with ethyl acetate / saturated brine solution. The resultant yellow solid was collected by filtration, washed with 2M hydrochloric acid, then dried under vacuum to give 15.5 g of the title compound. (LC/MS: Rt 2.92 [M+H]+ 250.89 ).

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 5334-40-7, its application will become more common.

3398-16-1, name is 4-Bromo-3,5-dimethylpyrazole, belongs to pyrazoles-derivatives compound, is considered to be a conventional heterocyclic compound, which is widely used in drug synthesis. The chemical synthesis route is as follows. Recommanded Product: 4-Bromo-3,5-dimethylpyrazole

General procedure: The corresponding pyrazole derivative 18, 19 or 22 (4 or 7 equiv) was dissolved in alkaline DMF [containing NaOH (4 or 7 equiv)] and the solution was stirred for 30 min at r.t. The bromomethyl-substituted benzene derivative 21 or 23 (1 equiv) was added and the reaction mixture was stirred for 24?48 h at 70 ¡ãC. The solution was cooled to r.t., then poured into ice water (50 mL), and the resulting precipitate was collected by filtration, washed thoroughly with H2O (3 ¡Á 15 mL) and dried in a desiccator.

The synthetic route of 3398-16-1 has been constantly updated, and we look forward to future research findings.

Reference of 35277-02-2, 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. 35277-02-2, name is 4-Fluoro-1H-pyrazole, This compound has unique chemical properties. The synthetic route is as follows.

Sodium hydride (13.8 g, 0.35 mol, 60% dispersion in mineral oil) was added to a solution of fluoropyrazole (20 g, 0.23 mol) in DMF (200 mL) 0 C. The mixture was stirred at room temperature for 1 h and then 2-bromo-ethanol (43 g, 0.35 mol) was added dropwisely at 0 C. The resulting mixture was stirred at 40 C. for 12 h. TLC (petroleum ether/EtOAc=1:1) indicated the reaction was complete. The mixture was quenched with saturated aqueous NH4Cl (200 mL). Then DMF was removed in vacuo and the residue was partitioned between Et2O (1000 mL) and H2O (1000 mL). The aqueous layer was extracted with more Et2O (4*1 L). The combined organic layers were dried over Na2SO4 and concentrated in vacuum to give compound 6c (20 g, 66%) as a yellow oil. 1H NMR (400 MHz, DMSO-d6) delta ppm 3.69 (t, J=5.56 Hz, 2H), 4.04 (t, J=5.56 Hz, 2H), 4.90 (br. s., 1H), 7.43 (d, J=4.29 Hz, 1H), 7.81 (d, J=4.55 Hz, 1H).

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

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. 15801-69-1, name is 4-Bromo-1,3,5-trimethyl-1H-pyrazole, A new synthetic method of this compound is introduced below., HPLC of Formula: C6H9BrN2

Step e: preparation of (2R,4S)-4-(tert-butyl-dimethyl-silanyloxy)-2-[hydroxy-(l,3,5- trimethyl-lH-pyrazol-4-yI)-methyl]-pyrrolidine-l-carboxylic acid benzyl ester[01 15] To a solution of 4-bromo-l,3,5-trimethyl- l H-pyrazole (950 mg, 5.0 mmol) in tetrahydrofuran (25 mL) is added n-butyllithium (2.1 mL, 2.5 M in hexane) at -78C and the resulting solution is stirred for 30 minutes. A solution of (2R,4S)-4-(tert-butyl-dimethyl- silanyloxy)-2-formyl-pyrrolidine-l -carboxylic acid benzyl ester (4 mmol) in tetrahydrofuran (5 mL) is added and the reaction mixture is slowly warmed to 0C over 30 minutes, stirred for 30 minutes, and quenched with ice water (40 mL). The organic layer is separated and the aqueous layer is extracted three times with ethyl acetate (60 mL). The combined organic phases are washed with a saturated sodium chloride solution, dried over magnesium sulfate, filtered and concentrated. The crude material is purified with a silica gel column chromatography (40-100% ethyl acetate/heptanes) to provide (2R,4S)-4-(tert-butyl-dimethyl-silanyloxy)-2-[hydroxy-(l,3,5- trimethyl-lH-pyrazol-4-yl)-methyl]-pyrrolidine- l -carboxylic acid benzyl ester (280 mg, 12%) as a light yellow oil. LC-MS: 474.1 (M+l).

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.