Day: April 19, 2021

Adding a certain compound to certain chemical reactions, such as: 35344-95-7, name is 1H-Pyrazole-4-carbaldehyde, 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 35344-95-7, Formula: C4H4N2O

A mixture of 8-(1 -methyl-1 H-indol-6-yl)-quinoxalin-6-ylamine (Intermediate 22) (100.00 mg; 0.34 mmol; 1 .00 eqr.), 1 H-pyrazole-4-carbaldehyde (41.89 mg; 0.44 mmol; 1.30 eg.) and CH3COOH (0.10 ml1.75 mmol; 5.22 eq.) in 1 ,2-dichloroethane (5.00 ml_) under argon at 5¡ãC is stirred for 10 min and next 1 h at rt. After this time, RM is cooled to 5¡ãC and NaBH(OAc)3 (96.80 mg; 0.44 mmol; 1.30 eq.) is added and then RM is stirred at rt overnight. RM is diluted with water and extracted with EtOAc. Combined organic layers are washed with brine, dried over Na2S04, filtered and evaporated. Brown residue is purified by FCC (DCM/MeOH; gradient) and repurified by preparative HPLC. 8-(1 -methyl-1 H-indol-6-yl)-N-(1 H-pyrazol-4- ylmethyl)quinoxalin-6-amine (55.00 mg; yield 46 percent; 99 percent by HPLC) 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, 1H-Pyrazole-4-carbaldehyde, other downstream synthetic routes, hurry up and to see.

These common heterocyclic compound, 29097-00-5, name is Methyl 3-amino-1H-pyrazole-4-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. Quality Control of Methyl 3-amino-1H-pyrazole-4-carboxylate

General procedure: A mixture of dialkyl malonate (10 mmol), anhyd toluene (25 mL), and N,N-dimethylformamide dimethylacetal (DMFDMA) (1.6 mL, 12 mmol) was heated under reflux for 2 h, cooled, and volatile components were evaporated in vacuo. The crude enamino ester 6 was dissolved in acetic acid (30 mL), aminopyrazole 3 (1.4 g, 10 mmol) was added and the mixture was heated under reflux for 5 h. The reaction mixture was cooled to rt and the precipitate was collected by filtration and washed with ethanol (2¡Á10 mL) to give the title compound 7. The following compounds were prepared in this manner.

The synthetic route of Methyl 3-amino-1H-pyrazole-4-carboxylate has been constantly updated, and we look forward to future research findings.

Related Products of 75415-03-1, 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 75415-03-1 as follows.

1st step: adding to the reaction kettle 2.1g2 – (1H-pyrazol-3-yl) pyridine and 3.7g2- bromopyridine [2 – (1H-pyrazol-3-yl) pyridine and 2-polybromide pyridine mole ratio of 1 : 1.6], in the reactor is placed into an oven after heating to 190 C, reaction 24h;2nd step: after the reaction is ended, take the solid using saturated Na2CO3solution cleaning, separating out the solid;3rd step: the separate the solid is dried fully then dissolved in chloroform, using silica gel as stationary phase, the volume of the petroleum ether and ethyl acetate ratio of 1:1 as the eluting agent mixed solution of dry-column, collecting product, evaporation and concentration, drying, the obtained yellow solid powder is the target product, nuclear product resonating chart as shown in Figure 1, the yield of 70.1%. The eluting agent is added before the dissolving solid petroleum ether for use out of the chloroform solution. he basic steps of the embodiment 1 the same, but in 1st step 2 – (1H-pyrazol-3-yl) pyridine and 2-bromo pyridine molar ratio of 1 : 1.5, the heating temperature is 180 C, the reaction time is 30h, saturation, solid in 2nd step NaHCO3solution cleaning, the obtained yield of 71.0%.

According to the analysis of related databases, 75415-03-1, the application of this compound in the production field has become more and more popular.

Electric Literature of 1280210-79-8, 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. 1280210-79-8 name is tert-Butyl 4,6-dihydropyrrolo[3,4-c]pyrazole-5(2H)-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.

Synthesis of 257-B and 258-B. To a solution of 257-A and 258-A (270 mg, 1.21 mmol) in DCM (6 mL) was added TFA (2 mL) dropwise under ice bath. Then the solution was stirred at room temperature 1 h. The solvent was removed in vacuo to give 257-B and 258-B as a crude product.Synthesis of 257-C and 258-C. A mixture of 257-B and 258-B (crude product from last step) and 143-C (286 mg, 0.61 mmol) in acetonitrile (10 mL) was stirred at 50 oC for 30 min, then Na2CO3 (581 mg, 6.05 mmol) was added into above mixture and stirred at 50 oC for 1 h. The mixture was cooled to room temperature. Na2CO3 was removed by filtered, the filtrate was concentrated in vacuo. The residue was purified by column chromatography on silica gel (DCM : MeOH = 200 : 1) to give 257-C (100 mg, 44%) as a yellow solid and 258-C (50 mg, 22%) as a yellow solid.

At the same time, in my other blogs, there are other synthetic methods of this type of compound, tert-Butyl 4,6-dihydropyrrolo[3,4-c]pyrazole-5(2H)-carboxylate, and friends who are interested can also refer to it.

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. COA of Formula: C6H8N2O3

Intermediate 17-65 (200 mg, 1.28 mmol) and POBr3 (500 mg, 1.74 mmol) are dissolved in MeCN (30 mL) and the resulting solution is heated in a sealed flask at 80 C for 3 h. The solution is cooled down and slowly poured into saturated NaHC03 solution (50 mL) and extracted with EtOAc. The combined extracts is washed with brine, dried over MgS04 and concentrated to afford intermediate 17-66 (200 mg).

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 51985-95-6, 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. 5203-77-0, name is 1,3-Dimethyl-1H-pyrazol-5-ol, A new synthetic method of this compound is introduced below., name: 1,3-Dimethyl-1H-pyrazol-5-ol

At room temperature, 1,3-dimethyl-1H-pyrazole-5-ol (0.65 g, 0.0058 mol) and (1.21 g, 0.012 mol) triethylamine were sequentially dissolved in 20 ml of dichloromethane.The low temperature bath was cooled to 3 C.To the above mixture was added dropwise 3-chloro-7-(methylsulfonyl)-5-(trifluoromethyl)quinoline-8-carbonyl chloride (2.23 g, 0.006 mol),The dropping rate was 4 drops / 30 seconds. After the addition was complete, the mixture naturally rose to room temperature and reacted for 5 hours.To the reaction mixture was added 10 ml of a saturated aqueous sodium hydrogen carbonate solution, and dichloromethane (3 * 15 ml) was extracted. The organic layers were combined, washed with water (1 * 15 ml), washed with saturated brine, and dried over anhydrous magnesium sulfate.The product was dissolved under reduced pressure to obtain 1.95 g of the product with a yield of 75%

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: 39806-90-1, name is 4-Iodo-1-methyl-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 39806-90-1, name: 4-Iodo-1-methyl-1H-pyrazole

g) Preparation of [0254] [0255] To a mixture of 4-iodo-1-methyl-1H-pyrazole (0.003 mol) and Cs2CO3 (1 g) was added 10 ml dioxane. The mixture was degassed by applying alternating N2 atmosphere and vacuum. Intermediate (66) (0.0022 mol) was added in 10 ml dioxane, and degassed as above. Pd2(dba)3 (0.1 g) and Xantphos (0.13 g) were added, degassed again, and the reaction mixture was stirred under a N2-atmosphere at 100 C. overnight. The reaction mixture was cooled, 150 ml water added, and extracted with 2 times with 150 ml of DCM. The combined organic layer was dried (MgSO4), filtered, and evaporated. The residue was purified by HPLC (HPLC method A). The residue was crystallized from DIPE, yielding 0.195 g of intermediate (67).

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, 4-Iodo-1-methyl-1H-pyrazole, 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. 1260243-04-6, name is Ethyl 5-amino-1H-pyrazole-4-carboxylate, A new synthetic method of this compound is introduced below., category: pyrazoles-derivatives

Step 3: preparation of ethyl 5-acetamido-1 H-pyrazole-4-carboxylate. A mixture of ethyl 5-amino-1H-pyrazole-4-carboxylate (100 g, 0.65 mol) and acetyl chloride (441.2 g, 5.62 mol) at 0C was heated to reflux for 4h. The reaction was concentrated in vacuo to remove excess acetyl chloride. Water (1.0 L) was added and the mixture was stirred for 16 h, after which it was filtered to afford the title compound as an off white solid (120g, 94%). MS (M+H) m/z 198. 1H NMR (400 MHz, CDCI3) 6 ppm: 9.57(1 H, s), 7.75 (1H, s), 4.33-4.28 (2H, q, J = 7.08), 2.27 (3H, s), 1 .37-1.34 (3H, s).

The synthetic route of 1260243-04-6 has been constantly updated, and we look forward to future research findings.

Application of 1353100-91-0,Some common heterocyclic compound, 1353100-91-0, name is Ethyl 3-bromo-1H-pyrazole-4-carboxylate, molecular formula is C6H7BrN2O2, 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.

[0506] to a solution of compound 32b (5.6 g, 25.57 mmol) in DMF(200 ml) was added mel (14.52 g, 102.28 mmol, 6.37 ml) andCs2CO3 (33.32 g, 102.28 mmol). The mixture was stirred at 25 C for 12 hrs. The mixture was diluted with H2O (1000 ml) and extracted with ethyl acetate (500 ml), then the organic layer was washed with brine (500 ml x 3), dried over Na2SO4 and concentrated. The residue (4 g) was purified by preparatory-hplc (basic condition). The residue was purified by column chromatography (SiO2, petroleum ether/ethyl acetate=10/l to 5: 1). Compound 32c (1g, yield: 16.8%) was obtained as a white solid. Compound 32d (2 g, yield: 33.6%) was obtained as a white solid.

The synthetic route of 1353100-91-0 has been constantly updated, and we look forward to future research findings.

Some common heterocyclic compound, 21230-50-2, name is 3-Amino-1-methyl-1H-pyrazole-4-carbonitrile, molecular formula is C5H6N4, 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

General procedure: Carbonitriles 7-10 (0.03 mol) was dissolved in 7 mL concdH2SO4 at 0 C and stirred at room temperature for 5 h. Then thereaction mixture was poured into ice cold water and neutralizedto pH 7 with 28% NH3 solution. The white precipitate was formedwhich was further washed with cold water and dried undervacuum.

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 21230-50-2, its application will become more common.