Day: March 5, 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. 288-13-1, name is 1H-Pyrazole, A new synthetic method of this compound is introduced below., category: pyrazoles-derivatives

3.40 g (0.05 mol) of pyrazoleAnd 2.8g (0.05mol) powdered KOH were added to a 100mL three-necked flask,Add 10mLDMSO as a solvent, the mixture was stirred at 80 for 30min,Then 6.25 g (0.05 mol) of 2-bromoethanol was added (added to the flask in 30 mL intervals, three times)Continue stirring for 20 ~ 30h, cooled to room temperature,After filtration, 20 mL of chloroform was added and the solution was washed with water (5 ¡Á 20 mL)Rotary drying to give a colorless transparent liquid 1-ethylpyrazole (yield: 60 ~ 70%).

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 of 175277-11-9, The chemical industry reduces the impact on the environment during synthesis 175277-11-9, name is 3-tert-Butyl-1-methylpyrazole-5-carboxylic Acid, I believe this compound will play a more active role in future production and life.

To a solution of 3-(t-butyl)-1-methyl-1H-pyrazole-5-carboxylic acid (0.054 g, 0.295 mmol) in dioxane (3 ml) was added TEA (0.123 ml, 0.885 mmol) followed by DPPA (0.095 ml, 0.442 mmol). The mixture was stirred at RT for 30 min and then treated with a solution of Example A3 (0.080 g, 0.295 mmol) in dioxane (3.00 ml). The reaction was then placed in an oil bath preheated to 100 C. and stirred with heating overnight. The completed reaction was cooled to RT. Without aqueous workup, the reaction mixture was purified directly by reverse phase chromatography (MeCN (w/0.1% TFA)/H2O (w/0.1% TFA)) to afford 1-(3-tert-butyl-1-methyl-1H-pyrazol-5-yl)-3-(2-fluoro-4-(2-(oxazol-2-yl)pyridin-4-yloxy)phenyl)urea of 96.8% purity. MS (ESI) m/z: 451.1 (M+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, 3-tert-Butyl-1-methylpyrazole-5-carboxylic Acid, other downstream synthetic routes, hurry up and to see.

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 20055-01-0 as follows. COA of Formula: C4H10N4O4S

To a solution of (2S)-2- [ (BENZYLOXYCARBONYL) AMINO]-6- [ (TERT- butoxycarbonyl) amino] hexanoic acid (19.02 g) and triethylamine (5.56 g) in tetrahydrofuran (200 ml) was added methyl chloroformate (4.21 ml), followed by stirring under ice-cooling for 30 minutes. To the reaction mixture was added a solution of 1-METHYL-LH- pyrazole-4,5-diamine sulfate (15.75 g) and triethylamine (15.2 g) in water (50 ml) at the same temperature. The mixture was stirred at room temperature for 30 minutes. To the reaction mixture was added chloroform (300 ml), and the layers were separated. The organic layer was washed successively with 10% aqueous citric acid solution, brine and saturated aqueous sodium hydrogencarbonate solution. The organic layer was dried over anhydrous magnesium sulfate, filtered and concentrated in vacuo to give a crude product of 1- benzyl 5-tert-butyl (lS)- {l- [ (5-amino-l-methyl-lH- pyrazol-4-yl) CARBAMOYL] PENTAMETHYLENE} biscarbamate as an oil. The crude product was used directly in the next step without further purification. To a solution of the crude product of 1-benzyl 5- tert-butyl (LS)-{1-[(5-AMINO-1-METHYL-LH-PYRAZOL-4- yl) CARBAMOYL] PENTAMETHYLENE} BISCARBAMATE IN. methanol (350 ml) was treated with 10% palladium on carbon (2.0 g) under a hydrogen atmosphere at room temperature for 6 days. After the catalyst was filtered off, the filtrate was concentrated in vacuo. The residue was triturated with ethyl acetate and dried in vacuo to give tert-butyl (5S)-5-amino-6- [ (5-amino-l-methyl-lH-pyrazol-4- yl) amino] -6-oxohexylcarbamate (12.1 g) as a solid. H-NMR (DMSO-D6) 6 1. 24-1. 40 (4H, m), 1. 36 (9H, s), 1. 70- 1.77 (2H, m), 2.88-2. 91 (2H, m), 3.51 (3H, s), 3.80-3. 82 (1H, m), 5.15 (2H, s), 6.77 (1H, br), 7.27 (1H, s), 10.05 (1H, br)

According to the analysis of related databases, 20055-01-0, the application of this compound in the production field has become more and more popular.

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. 39806-90-1, name is 4-Iodo-1-methyl-1H-pyrazole, This compound has unique chemical properties. The synthetic route is as follows., Safety of 4-Iodo-1-methyl-1H-pyrazole

General procedure: 4-Iodo-1-methyl-1H-pyrazole 1 (101 mg, 0.5 mmol) and phenylboronic 2 (59 mg, 0.5 mmol) were dissolved in DME (3 mL) and H2O (1.2 mL) in a microwave vial under a nitrogen atmosphere. Pd(PPh3)4 (2 mmol%, 11.6 mg) and Cs2CO3 (407.3 mg, 1.25 mmol) were added, and the reaction mixture was irradiated in a microwave apparatus at 90 C for 5-12 min. After the reaction mixture was cooled to ambient temperature, the product was concentrated, and the crude mixture was purified by silica gel column chromatography using petroleum ether/acetone as eluent to give the title compound.

According to the analysis of related databases, 39806-90-1, 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. 852227-86-2, name is 5-(Chloromethyl)-1,3-dimethyl-1H-pyrazole, A new synthetic method of this compound is introduced below., Computed Properties of C6H9ClN2

To a mixture of methyl ( 6-hydroxy-4-methyl-l- benzothiophen-3-yl) acetate (150 mg) and DMF (2 mL) were added 5- (chloromethyl) -1, 3-dimethyl-lH-pyrazole (101 mg) and K2C03 (175 mg). at room temperature. The mixture was stirred at room temperature for 3 h. The mixture was poured into water at room temperature and extracted with EtOAc. The organic layer was separated, washed successively with water and brine, dried over MgS04 and concentrated in vacuo. The residue was purified by silica gel column chromatography (EtOAc/hexane) . The product was crystallized from Et20-hexane to give the title compound (155 mg) . 1H NMR (300 MHz, CDC13) delta 2.26 (3H, s), 2.64 (3H, s) , 3.70-3.75 (3H, m) , 3.84 (3H, s) , 4.01 (2H, s) , 5.01 (2H, s), 6.10 (1H, s) , 6.76-6.81 (1H, m) , 7.10 (1H, s) , 7.23 (1H, d, J = 2.3 Hz).

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.

Electric Literature of 741717-63-5, A common heterocyclic compound, 741717-63-5, name is Ethyl 1-phenyl-3-(trifluoromethyl)-1H-pyrazole-4-carboxylate, molecular formula is C13H11F3N2O2, 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.

A mixture of ethyl l-phenyl-3- (trifluoromethyl) -IH- pyrazole-4-carboxylate (6.60 g, 23.2 mmol) and ethylenediamine (50 ml, 23.2 mmol) was heated at reflux for 3 hours. The mixture was concentrated under reduced pressure to a residue. To the residue was added toluene (50 mL) that was concentrate off, twice. The crude solid was dried under high vacuum overnight to give N- (2-aminoethyl) -l-phenyl-3-(trifluoromethyl) -lH-pyrazole-4-carboxamide (6.9 g, 99% yield) as a light tan solid. The desired product may also be isolated as the hydrochloride salt by dissolving in minimal DCM and adding IN HCl in Et2theta (3-5 molar equivalents) dropwise, filtering the solid and washing with Et2theta. 1H NMR (Free base analog) (DMSO-d6) delta 1.83 (br, 2H), 2.68 (t, J = 6.3 Hz, 2H), 3.21-3.26 (m, 2H), 7.47 (t, J = 7.4 Hz, IH), 7.60 (t, J = 8.0 Hzr 2H), 7.84 (d, J = 7.8 Hz, 2H), 8.29-8.30 (m, IH), 9.11 (s, IH); m/z (APCI pos) 299 (60%) (M+H) .

The synthetic route of 741717-63-5 has been constantly updated, and we look forward to future research findings.

Synthetic Route of 2075-45-8, These common heterocyclic compound, 2075-45-8, name is 4-Bromo-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.

4-Bromopyrazole (1. 0g, 6. [8MMOL)] and triethylamine (0. [90MOL,] 6. [5MMOL)] were stirred under nitrogen in DMF at [0C.] Trityl chloride (1.81g, 6. [5MMOL)] was added, and the mixture was stirred for two days at room temperature. The mixture was then diluted with chloroform (10 [ML),] and washed with water. The organic portion was dried over sodium sulphate and solvent evaporated in vacuo to give the crude product. The resulting solid was washed with di-isopropyl ether to give the title compound (1.55g) LCMS RT 4.09min, [CPh3] + 243

Statistics shows that 4-Bromo-1H-pyrazole is playing an increasingly important role. we look forward to future research findings about 2075-45-8.

Some common heterocyclic compound, 4149-06-8, name is 3-Amino-1-phenyl-1H-pyrazol-5(4H)-one, molecular formula is C9H9N3O, 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. Application In Synthesis of 3-Amino-1-phenyl-1H-pyrazol-5(4H)-one

General procedure: The mixture of alpha,beta-unsaturated ketone 1, or 4 (1.0 mmol), 3-amino-1-phenyl-1H-pyrazol-5(4H)-one 2 (1.0 mmol), p-TSAxH2O (0.3mmol), MeCN (4mL), H2O (4mL) was put in a reaction flask under 80 C about 1-3 h (monitored by TLC). After completion, the reaction mixture was cooled to room temperature and the products would be precipitated out at same time. Then, it was filtered, washed thoroughly with MeCN. The products were recrystallized from DMF.

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 4149-06-8, its application will become more common.

Some common heterocyclic compound, 27006-76-4, name is 5-Chloro-1,3-dimethyl-1H-pyrazole-4-carboxaldehyde, molecular formula is C6H7ClN2O, 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. name: 5-Chloro-1,3-dimethyl-1H-pyrazole-4-carboxaldehyde

General procedure: All reactions were carried out in vials under nitrogen atmosphere. Step 1: A solution of compound 8 (100 mumol, 1.0 equiv) and compound 9 (150 mumol, 1.5 equiv) in DMF (0.1 M) was treated with K2CO3 (300 mumol, 3.0 equiv) and stirred at 110 C for 16 h (LCMS check). The reaction was filtered and the filtrate concentrated to afford 10. The crude aldehyde 10 (100 mumol, 1.0 equiv) was dissolved in acetone:water (2:1, 0.1 M) and treated with KMnO4 (600 mumol, 6 equiv) and stirred at 30 C for 16 h (LCMS check). The reaction was filtered and the filtrate concentrated to afford 11. The crude acid 11 (100 mumol, 1.0 equiv) was treated with HATU (120 mumol, 1.20 equiv) followed by the crude amine (100 mumol, 1.0 equiv) and NEt3 (300 mumol, 3.0 equiv). The reaction was stirred at 30 C for 16 h (LCMS check). The reactions were concentrated and purified directly by reversed phase preparative HPLC using a C18 column and eluting with acetonitrile-water (0.225% formic acid or pH = 10 NH4OH) gradient. All compounds were deemed greater than 95% purity by LCMS and HPLC.

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 27006-76-4, its application will become more common.

Some common heterocyclic compound, 288148-34-5, name is 1-Methyl-1H-pyrazole-4-sulfonyl chloride, molecular formula is C4H5ClN2O2S, 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. category: pyrazoles-derivatives

Dissolve [2-(3′-chloro-2,3,5,6-tetrahydro-[l,2′]bipyrazinyl-4-yl)-ethyl]-methyl- amine hydrochloride salt (1.0 g, 2.57 mmol) in dichloromethane (20 ml) and cool in an ice-bath. Add triethylamine (1.79 ml, 12.87 mmol) and then 1 -methyl pyrazole-4- sulfonyl chloride (465 mg, 2.57 mmol). Remove the ice-bath and allow to warm to ambient temperature and allow to stir for 20 hr. Wash the combined organic layers with aqueous sodium bicarbonate, brine and water. Dry over sodium sulfate and concentrate. Purify by chromatography, eluting with 1:2 hexanes: acetone to afford the title compound (1.1 g, 97 % yield) as a white foam. MS ES: m/z = 400 [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 288148-34-5, its application will become more common.