Month: April 2021

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. 84547-84-2, name is 4-Bromo-1-methyl-1H-pyrazole-5-carboxylic acid belongs to pyrazoles-derivatives compound, it is a common compound, a new synthetic route is introduced below. SDS of cas: 84547-84-2

To a solution of N-methyl-4-bromopyrazole-3-carboxylic acid (2.0 g), available from step A, in 65 mL of anhydrous DMF was added bromotripyrrolidinophosphonium hexafluorophosphate (PyBrop, 4.60 g), dimethyl amine (10 mL, 2.0 M in THF) and diisopropylethyl amine (5.2 mL) at 25 C. The mixture was stirred for 26 h, and concentrated under reduced pressure to an oily residue. This residue was treated with a 1.0 M NaOH aqueous solution, and extracted with ethyl acetate (50 mL?4). The organic extracts were combined, washed with brine, and dried with anhydrous Na2SO4. Removal of solvents yielded an oil, which was purified by preparative thin layer chromatography, eluting with CH2Cl2-MeOH (20:1), to give 1.09 g of the amide product (48%, MH+=232.0).

The synthetic route of 84547-84-2 has been constantly updated, and we look forward to future research findings.

Synthetic Route of 1203705-55-8, These common heterocyclic compound, 1203705-55-8, name is 3-Bromo-1H-pyrazol-5-amine, 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: 1H-Pyrazol-5-amine 1 (1 equiv.), 3-oxopropanenitrile 2 (1 equiv.), benzaldehyde 3 (1 equiv.), and Et3N (2 equiv.) were stirred in DMF (1 M) at 90 C for 16 h. The volatiles were removed under reduced pressure (or positive N2 (g) pressure). Sodium nitrite (3 equiv.) and acetic acid (134 equiv.) were added to the crude material, and the reaction mixture was stirred for 10 min. The volatiles were removed under reduced pressure (or positive N2 (g) pressure), and the crude reaction mixture was subjected to silica gel column chromatography with ethyl acetate in hexanes.

The synthetic route of 1203705-55-8 has been constantly updated, and we look forward to future research findings.

Related Products of 930-36-9, These common heterocyclic compound, 930-36-9, name is 1-Methylpyrazole, 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.

Phosphorus oxychloride (6.92 g, 45.1 mmol, 1.50 equiv.) was cooled to 0 0C and then added drop-wise to anhydrous DMF (3.50 mL, 45.2 mmol, 1.50 equiv.) at 0 0C. The mixture was stirred 1 hour at room temperature and was then heated to 80 0C. The compound of formula VIII (2.50 mL, 30.2 mmol) was then added drop-wise to the reaction, and the resulting mixture was stirred 3 hours at 95 0C. The reaction was then quenched by slow addition to ice (40 g). The pH of the resulting solution was 2, and it was raised to 5 by slow addition of 12N aqueous sodium hydroxide solution (11.2 mL). The resulting aqueous solution was extracted with dichloromethane and/or ether (7 x 40 mL), and additional sodium hydroxide was added during extraction, as needed, to maintain a pH of 5. The extracts were then combined, dried over sodium sulfate, filtered and concentrated to yield a brown oil (3.79 g, 59% yield).

The synthetic route of 930-36-9 has been constantly updated, and we look forward to future research findings.

Some common heterocyclic compound, 930-36-9, name is 1-Methylpyrazole, molecular formula is C4H6N2, 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 1-Methylpyrazole

Step 1) Method A: Phosphorus oxychloride (6.92 g, 45.1 mmol, 1.5 eq.) was cooled to 0C and then added drop- wise to anhydrous DMF (3.50 mL, 45.2 mmol, 1.5 eq.) at 0C. The colorless DMF solution soon becomes orange. The mixture was stirred for 1 hour at room temperature and then heated to 80C. 1 -Methyl- IH-pyrazole (2.5 mL, 30.2 mmol) is then added drop-wise to the reaction, and the resulting mixture was stirred 3 hours at 95C. The reaction was then quenched by slow addition to ice (40 g) via Pasteur pipette. The pH of the resulting solution was 2, and it was raised to 5 by slowly adding 12N aqueous sodium hydroxide solution (11.2 mL total). The resulting aqueous solution was extracted with dichloromethane (3 x 40 mL). At this point, the pH of the aqueous layer had dropped to 3, therefore additional 12 N NaOH solution (1 mL) was added to bring the pH to 6. The aqueous layer was then extracted further with ether (4 x 40 mL). The combined extracts were then dried over sodium sulfate, filtered and concentrated (at about 40-50C). After drying for 30 minutes under vacuum, a brown oil was recovered (3.79 g) which NMR indicated consisted of a mixture of product, starting material and DMF (52 wt %, 22 wt %, and 26 wt %, respectively). The calculated yield of was 59% and the calculated yield for recovery of unreacted starting material, was 34%. This crude material may be used without further purification in the next step.

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 930-36-9, 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. 138907-68-3, name is Ethyl 5-amino-1-(4-fluorophenyl)-1H-pyrazole-4-carboxylate, This compound has unique chemical properties. The synthetic route is as follows., Product Details of 138907-68-3

Intermediate 9: 5-Amino-1-(4-fluorophenyl)-1 H-pyrazole-4-carboxylic acid. To a suspension of ethyl 5-amino-1-(4-fluorophenyl)-1 H-pyrazole-4-carboxylate (12.1g, 48.5mmol) in ethanol (250ml) was added a solution of lithium hydroxide(5.8g, 242mmol) in water (100ml). The mixture was stirred at reflux for 2.5hr. It was allowed to cool and concentrated to 50% of its volume before 5M hydrochloric acid(47ml) was added. After stirring for 15mins, the resulting white solid was filtered off and further 5M hydrochloric acid (3ml) was added. This was filtered and the combined solids were washed with water and diethyl ether and then dried under vacuum to give the title compound (10.27g).1 H NMR (400 MHz, DMSO-d6) deltappm 12.09 (br. s., 1 H) 7.67 (s, 1 H) 7.54 – 7.60 (m, 2H) 7.34 – 7.41 (m, 2 H) 6.29 (br. s., 2 H).LC-MS Retention Time 2.20mins, MH+ 222.

According to the analysis of related databases, 138907-68-3, the application of this compound in the production field has become more and more popular.

Adding a certain compound to certain chemical reactions, such as: 16034-46-1, name is 1-Methyl-1H-pyrazole-5-carboxylic 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 16034-46-1, Application In Synthesis of 1-Methyl-1H-pyrazole-5-carboxylic acid

To a solution of tert-butyl [2-(3,5-difluorobenzyl)-4-methyl-1,3-thiazol-5-yl]carbamate (300 mg, 0.881 mmol) obtained in Example 220-D) in ethanol (2 mL) was added dropwise concentrated hydrochloric acid (0.630 mL) at room temperature, and the mixture was stirred at 50C for 3.5 hr. The reaction mixture was cooled to 0C, neutralized with 8N aqueous sodium hydroxide solution, adjusted to pH 10-11 with saturated aqueous sodium hydrogen carbonate solution, and extracted with ethyl acetate. The organic layer was dried over anhydrous magnesium sulfate and concentrated under reduced pressure. The obtained residue was dissolved in DMA (8 mL), and 1-methyl-1H-pyrazole-5-carboxylic acid (134 mg, 1.06 mmol), HATU (403 mg, 1.06 mmol) and DIEA (0.0728 mL, 0.441 mmol) were added at room temperature. The reaction mixture was stirred at 60C for 3.5 hr, cooled to room temperature, water and 0.1N hydrochloric acid were added and the mixture was extracted with ethyl acetate. The organic layer was washed with saturated aqueous sodium hydrogen carbonate solution and saturated brine, dried over anhydrous magnesium sulfate, and concentrated under reduced pressure. The obtained residue was purified by silica gel column chromatography [eluent: hexane-ethyl acetate (3:2-3:7)] and basic silica gel column chromatography [eluent: hexane-ethyl acetate (3:2-3:7)], and crystallized from ethyl acetate-hexane to give the title compound (144 mg) as colorless crystals (yield 47%). MS (ESI+): [M+H]+ 349. 1H NMR (300 MHz, DMSO-d6) delta 2.31 (3H, s), 4.05 (3H, s), 4.26 (2H, s), 7.04-7.17 (4H, m), 7.54 (1H, d, J = 2.3 Hz), 10.53 (1H, s).

At the same time, in my other blogs, there are other synthetic methods of this type of compound, 1-Methyl-1H-pyrazole-5-carboxylic acid, and friends who are interested can also refer to it.

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. 73387-46-9, name is 3-(4-Bromophenyl)-1H-pyrazole belongs to pyrazoles-derivatives compound, it is a common compound, a new synthetic route is introduced below. Product Details of 73387-46-9

Production Example 138 3-(4-Bromophenyl)-1-trityl-1H-pyrazole 32.71 g of the title compound was obtained as pale brown crystals from 6.74 g 3-(4-bromophenyl)-1H-pyrazole (compound in Production Example 125) by the same method as in Production Example 15.1H-NMR (CDCl3) delta: 6.51(d, J=2.4Hz, 1H), 7.20(m, 6H), 7.29(m, 10H), 7.45(d, J=8.8Hz, 2H), 7.65(d, J=8.8Hz, 2H)

The synthetic route of 73387-46-9 has been constantly updated, and we look forward to future research findings.

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. 15802-75-2, name is 4-Iodo-3-methyl-1H-pyrazole belongs to pyrazoles-derivatives compound, it is a common compound, a new synthetic route is introduced below. COA of 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 mmol2-iodo-5- (2-iodopyrimidine-3) pyrimidine, 2.0 mmol of 3-methyl-4-iodopyrazole, 0.03 mmol of palladium acetate,0.05 mmol di-t-butyl (2 ‘, 4′, 6′-triisopropyl-3,6-dimethoxybiphenyl-2-yl)4.0 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, 3.0 mmol of 4-carboxyphenylboronic acid, 0.02 mmol of palladium acetate, 0.04 mmol2′-dicyclohexyl-2,6-dimethoxy-3-sulfonic acid-1,1’-biphenyl sodium salt, 7.0 mmol sodium carbonate,And 100 mmol of water; then heated to 100 C with an oil bath under magnetic stirring and the reaction was refluxed for 24 hours.Down to room temperature; add 20 ml of water, filtration, with concentrated hydrochloric acid to adjust the pH of the filtrate to 1, room temperature stirring 3h,Filtered, washed with ethanol, dried product 16, yield 72%. The product (C30H22N8O4)Of the mass spectrum (ESI) of 558.20.

The synthetic route of 15802-75-2 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. 155377-19-8, name is Ethyl 3-(trifluoromethyl)pyrazole-4-carboxylate, A new synthetic method of this compound is introduced below., Formula: C7H7F3N2O2

According to the procedure of Buchwald et al . (J. Oxg. Chem. 2004, 69, 5578), to a 350 iaL sealed tube flushed vigorously with nitrogen was added ethyl 3- (trifluoromethyl) – lH-pyrazole-4-carboxylate (20.0 g, 96.1 mmol) , 1-iodobenzene (12.9 inL, 115 mmol), potassium carbonate (27.9 g, 202 mmol), copper(I) iodide (0.915 g, 4.80 mmol), and (IS, 2S) -N1,N2- dimethylcyclohexane-l,2-diamine (1.37 g, 9.61 mmol), followed by degassed (argon) toluene (100 mL) . The mixture was stirred for 24 hours at 1100C, cooled to room temperature, and filtered through a short silica pad which was thoroughly rinsed with toluene and AcOEt- The filtrate was concentrated in vacuo to give ethyl l-phenyl-3- (trifluoromethyl) -lH-pyrazole-4- carboxylate (21 g, 77%) as a solid: 1H NMR (400 MHz, CDCl3) delta 1.39 (t, 3H, J = 7.0 Hz), 4.37 (q, 2H, J = 7.0 Hz), 7.42 (m, IH), 7.52 (m, 2H), 7.72 (m, 2H), 8.48 (m, IH).

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.

Related Products of 13599-12-7, These common heterocyclic compound, 13599-12-7, name is Ethyl 3-phenyl-1H-pyrazole-5-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.

Ethyl 2,4-dioxo-4-phenylbutanoate (16b) (2.6 g, 9.1 mmol)Dissolved in 30mL of methanol, added 15mL lithium hydroxide monohydrate(0.5 g, 20.0 mmol) in water. The reaction was heated to 70 C until the hydrolysis was complete. Concentration under reduced pressure gave a solid suspension. 15 mL of water was added and the pH was adjusted to 3 with 1 N diluted hydrochloric acid. Filtering,The title compound 5-phenyl-1H-pyrazole-3-carboxylic acid (Intermediate 16) was obtained.Dark white solid (2.1 g, yield 89.5%).

Statistics shows that Ethyl 3-phenyl-1H-pyrazole-5-carboxylate is playing an increasingly important role. we look forward to future research findings about 13599-12-7.