Day: April 8, 2021

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 35277-02-2 as follows. Safety of 4-Fluoro-1H-pyrazole

Add in 100mL round bottom flask1-bromo-N- (6-cyano-5-trifluoromethyl-pyridin-3-yl) -cyclobutanecarboxamide (0.30 g, 0.8618 mmol),4-fluoro-1H-pyrazole (0.148 g, 1.7236 mmol),Cuprous bromide dimethyl sulfide (17.7 mg, 0.08618 mmol),Triphenylphosphine (22.6 mg, 0.08618 mmol),Tripotassium phosphate (0.22 g, 1.0341 mmol),Sodium hydroxide (38 mg, 0.9480 mmol),10mL of anhydrous toluene was used as the solvent.The resulting mixture was heated to 50 C,Stir for 15 hours under argon protection.After confirming the completion of the reaction by thin layer chromatography,The reaction solution is cooled to 20 ¡À 5 ,Then add water (30 ml) and ethyl acetate (35 ml),After brief stirring, the liquid is separated,The organic phase was washed with brine (25 ml),Magnesium sulfate drying,filter,Drain the organic phase,An oily substance is obtained.Silica gel column chromatography separation (mobile phase is dichloromethane: ethyl acetate = 9: 1), purification,82 mg of yellow powder was obtained,Identified asN- (4-cyano-3-trifluoromethyl) phenyl-1- (4-fluoro-1H-pyrazol-1-yl) -cyclobutanecarboxamide.The yield is 27%.

According to the analysis of related databases, 35277-02-2, the application of this compound in the production field has become more and more popular.

Electric Literature of 288148-34-5, These common heterocyclic compound, 288148-34-5, name is 1-Methyl-1H-pyrazole-4-sulfonyl chloride, 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 2 1-Methyl-1H-pyrazole-4-sulfonic acid 4-[2-(4-bromo-benzyl)-4,5-dimethyl-thiophene-3-carbonyl]-2-cyclopentyl-phenyl ester At ambient temperature, to a stirred solution of [2-(4-bromobenzyl)-4,5-dimethyl-thiophen-3-yl]-(3-cyclopentyl-4-hydroxy-phenyl)-methanone (0.283 g, 0.603 mmol) in N,N-DMF (3.0 mL) was added 60% sodium hydride/mineral oil (24.1 mg, 0.603 mmol). After 0.5 h, to the reaction was added a solution of 1-methyl-1H-pyrazole-4-sulfonyl chloride (0.120 g, 0.664 mmol) in N,N-DMF (1.3 mL). After 3 h, the reaction was quenched with 1N NaOH (40 mL), extracted with CH2 Cl2, dried (Na2 SO4) and concentrated. Purification on Biotage KP-Sil eluding with 20% acetone/hexane gave 0.202 g (55%) of the title compound as a yellow solid, mp 55-60 C. (DMSO-d6) delta 1.29-1.34 (m, 2 H), 1.59-1.79 (m, 6 H), 1.81 (s, 3 H), 2.28 (s, 3 H), 3.08 (quintet, 1 H), 3.87 (s, 2 H), 3.89 (s, 3 H), 6.98 (d, 2 H), 7.32 (d, 1 H), 7.39 (d, 2 H), 7.53-7.57 (m, 2 H), 7.97 (s, 1 H), 8.62 (s, 1 H). IR (KBr) 3450, 2950, 1650, 1490, 1400, 1370 and 1170 cm-1. mass spectrum (+ESI) m/z 613/615 (M+H).

The synthetic route of 288148-34-5 has been constantly updated, and we look forward to future research findings.

Related Products of 5334-43-0, A common heterocyclic compound, 5334-43-0, name is 5-Amino-1-phenyl-1H-pyrazole-4-carbonitrile, molecular formula is C10H8N4, 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.

General procedure: To a stirred solution of the intermediate compounds 1a-1d (1 mmol) and triethylamine (2 mmol) in DMF (12 mL) medium, a mixture of EDCI (1 mmol) and HOBt (1mmol) was added and the reaction mixture was stirred at room temperature for 30 min, then a mixture of compounds 2a-2d (1 mmol) and DMF (5 mL) was added, the reaction was stirred at room temperature. And the reaction progress was monitored by TLC. After completion of the reaction, the product was added into chloroform, then extracted from chloroform with water, and washed successively with 0.2 mol/L hydrochloric acid, water,2 mol/L sodium hydroxide, water, saturated sodium chloride, then dried, concentrated and purified by preparative thin layer chromatography (PE:EA = 8:1) followed by recrystallization from ethanol.

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.

Adding a certain compound to certain chemical reactions, such as: 42098-25-9, name is 5-Chloro-1-methyl-4-nitro-1H-pyrazole, 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 42098-25-9, Formula: C4H4ClN3O2

Example 354 5-amino-2-(2,6-difluorophenyl)-N-[1-methyl-5-(9-oxa-3,7-diazabicyclo[3.3.1]nonan-3-yl)pyrazol-4-yl]thiazole-4-carboxamide 354 [1008] RRN No.1703,1706,1708,1710Step A. To a microwave reaction vial was added 5-chloro-1-methyl-4-nitro-1H-pyrazole (141 mg, 0.88 mmol), tert-butyl 9-oxa-3,7-diazabicyclo[3.3.1]nonane-3-carboxylate (200 mg, 0.88 mmol). Ethanol (8 mL) and diisopropylethylamine (0.92 mL, 5.25 mmol) were added and the mixture was irradiated with a microwave for 60 min at 130 C. The mixture was cooled, concentrated and purified via flash chromatography, ethyl acetate/ heptane 0% to 100% to afford yellow oil tert-butyl 7-(2-methyl-4-nitro-pyrazol-3-yl)-9-oxa-3,7-diazabicyclo[3.3.1]nonane-3-carboxylate (202 mg, 65%).

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-Chloro-1-methyl-4-nitro-1H-pyrazole, other downstream synthetic routes, hurry up and to see.

Electric Literature of 694-31-5,Some common heterocyclic compound, 694-31-5, name is 1,5-Dimethyl-1H-pyrazole, molecular formula is C5H8N2, 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.

In this example, the preparation of 1,5-dimethylpyrazole hydrobromide is as follows:1.442 g (15 mmol) of 1,5-dimethylpyrazole and 3.102 g (18 mmol) of hydrobromic acid were respectively added to 100 mL of three neck Bottle, stirring 15 ~ 30h; After the reaction, the addition of water, the product was washed with ethyl acetate and dried to give a white solid 1,5-dimethylpyrazole hydrobromide ionic liquid, a yield of 70%

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 1,5-Dimethyl-1H-pyrazole, its application will become more common.

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. 15802-75-2, name is 4-Iodo-3-methyl-1H-pyrazole, A new synthetic method of this compound is introduced below., Formula: C4H5IN2

Under nitrogen protection,To a 10 ml Schlek reaction tube (a glass instrument commonly used in anhydrous oxygenless operation) was added 1.0 mmolBromo-5- (4- (6-bromopyridyl-3) phenyl) pyridine, 2.2 mmol3-methyl-4-iodopyrazole,0.03 mmol of palladium acetate, 0.05 mmol of di-t-butyl (2 ‘, 4′, 6′-triisopropyl-3,6-dimethoxybiphenyl-2-yl) phosphine, 6.0 mmol of sodium tert-butoxide ,And 5 ml of toluene,The reaction tube was purged with nitrogen three times,And then heated to 110 C with an oil bath under magnetic stirring, and the reaction was refluxed for 24 hours. Down to room temperatureThe reaction solution was further added, 4.0 mmol of 4-carboxyphenylboronic acid, 0.03 mmol of palladium acetate,0.06 mmol 2′-dicyclohexylphosphino-2,6-di-I-propyl-4-sulfonate-1,1’-biphenyl sodium,8.0 mmol of potassium carbonate, and 100 mmol of water; and then heated to 100 C with an oil bath under magnetic stirring,The reaction was refluxed for 40 hours. Down to room temperature; add 20 ml of water, filtration, with concentrated hydrochloric acid to adjust the pH of the filtrate to 1,After stirring at room temperature for 3 h, the mixture was filtered, washed with ethanol and dried to obtain product 21, yield 77%.The mass spectrum (ESI) data for this product (C38H28N6O4) was 632.26.

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 309740-49-6, A common heterocyclic compound, 309740-49-6, name is Methyl 1-methyl-4-nitro-1H-pyrazole-5-carboxylate, molecular formula is C6H7N3O4, 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.

1-methyl-4-nitro-1H-pyrazole-5-carboxylate(1.0 g, 5.4 mmol) was dissolved in methanol (30 mL)Palladium on carbon (100 mg),Access to hydrogen,25 C for 3 hours,filter,The filtrate was concentrated in vacuo to give the product(0.8 g, yield: 95.2%).

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 930-36-9, 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. 930-36-9, name is 1-Methylpyrazole belongs to pyrazoles-derivatives compound, it is a common compound, a new synthetic route is introduced below.

2-Methyl-2H-pyrazole-3-boronic acid: N-methyl pyrazole (25 mL, 0.3 mol) was dissolved in 500 mL of THF. The solution was then cooled to-78C in a dry ice/isopropanol bath. Once the solution reached -78C, n-BuLi (140 mL, 0.40 mol) was added dropwise by canula. The reaction mixture was stirred at -78C for 1.5 hours. Then, triisopropyl borate (280 mL, 1.2 mol) was added to the above mixture via canula. While stirring overnight, the reaction temperature was gradually increased from -78deltaC to 0deltaC. The pH of the mixture was adjusted to 6 with IN HCI. THF was removed under reduced pressure, and the aqueous residue was extracted with EtOAc (2 x 100mL). The solid was then filtered to yield 108 g (100%) of 2-methyl-2H-pyrazole-3-boronic acid as a yellow solid.

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, 1-Methylpyrazole, other downstream synthetic routes, hurry up and to see.

Synthetic Route of 51985-95-6,Some common heterocyclic compound, 51985-95-6, name is Methyl 5-hydroxy-1-methyl-1H-pyrazole-3-carboxylate, molecular formula is C6H8N2O3, 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.

Intermediate 43a) Methyl 5-hydroxy-1 -methyl-1 H-pyrazole-3-carboxylate (2.0 g) was added at 0 ¡ãC to a solution of phosphorus(V) oxychloride (13.7 g) in dry DMF (3 g) and the mixture was heated to 120 ¡ãC for 4 h. After cooling to ambient temperature the reaction was quenched by the addition of ice water (100 mL) and the suspension was stirred for 30 min. The precipitated solid formed was isolated through filtration and was washed with water to yield the desired compound (56percent yield). LC-MS (Method 2): mlz [M+H]+ = 203.2 (MW calc. = 202.60); R, = 2.3 min.

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route Methyl 5-hydroxy-1-methyl-1H-pyrazole-3-carboxylate, its application will become more common.

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. 39806-90-1, name is 4-Iodo-1-methyl-1H-pyrazole, A new synthetic method of this compound is introduced below., Safety of 4-Iodo-1-methyl-1H-pyrazole

To a solution of 3-iodo-l-methyl-lH-pyrazole (20 mg, 0.096 mmol) and intermediate C.5 (20 mg, 0.074 mmol) in anhydrous l,4-Dioxane (1 ml) was added (Irans)-N I .N2-dimethylcyclohexane- 1, 2-diamine (5 mg, 0.035 mmol), Cul (5 mg, 0.026 mmol) and K3PO4 (50 mg, 0.236 mmol). The resulting mixture was stirred at 90C for 16 hours. After filtering and concentrating the reaction solution, the residue was purified by prep-HPLC (basic) to afford example 6.1, 5-methyl-l-(l- methyl-lH-pyrazol-4-yl)-6-(l-(oxetan-3-yl)piperidin-4-yl)-lH-indazole. MS (ESI) m/z calc?d for C20H26N5O [M+H]+ 351, found 351. -NMR (500 MHz, CDC13) d 8.00 (s, 1H), 7.82 (s, 1H), 7.73 (s, 1H), 7.53 (s, 1H), 7.42 (s, 1H), 4.66-4.71 (m, 4H), 4.02 (s, 3H), 3.51-3.57 (m, 1H), 2.92 (m, 2H), 2.85 (m, 1H), 2.45 (s, 3H), 1.97-2.02 (m, 2H), 1.87 (m, 4H). LRRK2 IC50 1.1 nM.

The synthetic route of 39806-90-1 has been constantly updated, and we look forward to future research findings.