Tag: M.W:100-200

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.

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.

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.

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.

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.

139756-02-8, name is 4-Amino-1-methyl-3-N-propyl-1H-pyrazole-5-carboxamide, 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. category: pyrazoles-derivatives

General procedure: To a solution of 2-aminobenzamide (1.470 mmol, 1.0 eq.) was added to a solution of Terminal Alkyne (1.470 mmol, 1.0 eq.), Tosyl Azide, (1.470 mmol, 1.0eq.), CuI (0.147 mmol, 0.1 eq.), triethylamine (2.941 mmol, 2.0 eq.), in acetonitrile (10 ml) under N2 atmosphere. The mixture was stirred at room temperature for 12 h. After completion of the reaction (as indicated by TLC) the reaction mixture was poured into water (25 mL) and extracted with ethyl acetate (2×25 mL), dried over Na2SO4, concentrated under vacuum to get crude compound which was purified by column chromatography using a mixture of petroleum ether: ethyl acetate to give the desired product as a white solid.

The synthetic route of 139756-02-8 has been constantly updated, and we look forward to future research findings.

Related Products of 1572-10-7,Some common heterocyclic compound, 1572-10-7, name is 3-Amino-5-phenylpyrazole, molecular formula is C9H9N3, 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: The compound tetronic acid (15) (80 mg, 0.8 mmol) was dissolved in 4 mL of ethanol, followed by addition of terphenyl aldehyde 13a (221.2 mg, 0.8 mmol) and 3-amino-5-phenyl pyrazole 14a (127.2 mg, 0.8 mmol). The reaction mixture was refluxed in ethanol at 78 C for an hour. Then reaction suspension was cooled to room temperature, and the precipitated product was collected by vacuum filtration and washed with ethanol (3 mL), then recrystallized from ethanol to afford pure compound 8a as a white solid, 340 mg in 85% yield. Mp: 273-274 C; 1H NMR (300 MHz, DMSO-d6): delta 4.80 (s, 2H), 5.25 (s, 1H ), 6.89-6.99 (m, 1H), 7.19-7.35 (m, 7H), 7.42-7.52 (m, 4H), 7.65 (dd, 4H, J = 8.8, 11.7 Hz), 8.05 (s, 1H), 10.19 (s, 1H ), 12.56 (s, 1H); 13C NMR (300 MHz, DMSO-d6): delta 30.5, 64.8, 94.4, 99.8, 111.1, 111.3, 113.2, 121.3, 125.4, 126.1, 126.7, 126.9, 127.1, 127.2, 127.3, 128.3, 128.7, 128.8, 132.7, 137, 137.2, 138.8, 139.3, 145.8, 152.7, 157.7, 172.2; MS (ESI): 500 [M+H]+; HRMS (ESI) calcd for C32H23O2N3F [M+H]+ 500.1712; found: 500.1738.

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 3-Amino-5-phenylpyrazole, its application will become more common.

Electric Literature of 1369959-12-5, 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. 1369959-12-5, name is 3-Chloro-5-nitro-1H-pyrazole, This compound has unique chemical properties. The synthetic route is as follows.

General procedure: To a solution of 3-methyl-5-nitro-lH-pyrazole (2.46 g, 19.40 mmol) and l -methyl-4- piperidinemethanol (5.00 g, 38.70 mmol) in dry Me-THF (190 mL). Di-tert-butyl azodicarboxylate (8.91 g, 38.70 mmol) and PPh3 (10.20 g, 38.70 mmol) were added. The solution was heated at 55 C over the weekend. The reaction mixture was diluted with EtOAc and water. The organic layer was separated and the aqueous layer was extracted thrice with EtOAc. The organic layers were combined, washed with brine, dried over MgS04, filtered and concentrated. The residue (yellow oil) was purified by column chromatography on silica gel (Irregular SiOH, 15-40 muiotaeta, 330 g, liquid loading in DCM, mobile phase: DCM/MeOH, gradient from 100:0 to 90: 10). The fractions containing the product were combined and evaporated to dryness to give 2.36 g of intermediate 195 (51% yield, yellow oil).

The chemical industry reduces the impact on the environment during synthesis 3-Chloro-5-nitro-1H-pyrazole. I believe this compound will play a more active role in future production and life.

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. 3112-31-0, name is 1H-Pyrazole-3,5-dicarboxylic acid belongs to pyrazoles-derivatives compound, it is a common compound, a new synthetic route is introduced below. HPLC of Formula: C5H4N2O4

A. 5-[(R)-2-Biphenyl-4-yl-1-(1-carboxy-cyclopropylmethyl)-ethylcarbamoyl]-2H-pyrazole-3-carboxylic acid (R7 = H) 3,5-Pyrazoledicarboxylic acid (35.2 mg, 226 mumol, 1.0 eq.), DIPEA (126 muL) and HATU (85.9 mg, 226 mumol, 1.0 eq.) and DCM (5 mL) were combined and stirred for 5 minutes at room temperature. 1-((R)-2-Amino-3-biphenyl-4-yl-propyl)-cyclopropanecarboxylic acid (86.7 mg, 294 mumol, 2.3 eq,) and DIPEA (0.5 mL) in DCM (5 mL) was added, and the resulting mixture was stirred for 1 hour. The reaction was quenched with saturated aqueous NH4Cl and the product was extracted with DCM, dried and evaporated. The resulting product was combined with AcOH (1.5 mL) and purified with preparative HPLC to yield the title compound (21.4 mg; 93percent purity). MS m/z [M+H]+ calc’d for C24H23N3O5, 434.16; found 433.5.

The synthetic route of 3112-31-0 has been constantly updated, and we look forward to future research findings.

Electric Literature of 1018446-95-1, 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. 1018446-95-1 name is tert-Butyl 4-amino-1H-pyrazole-1-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.

To a microwave tube was added 4-bromo-2-(2, 6-dichlorophenyl)-lH-imidazo-[4,5- c]-pyridine (0.050 g, 0.15 mmol), tert-butyl-4-amino-lH-pyrazole-l-carboxylate (0.032 g, 0.17 mmol), Pd2(dba)3 (0.013 g, 0.015 mmol), XantPhos (0.017 g, 0.03 mmol), Cs2C03 (0.098 g, 0.03 mmol) and dioxane (1.2 niL). The mixture was degassed with N2 for 1 min. The resulting mixture was irradiated in a microwave reactor at 160 C for 2 housr and then cooled to room temperature. The mixture was filtered with Celite and the filtrate was concentrated by vacuum. The residue was purified by prep-HPLC (Gilson GX 281 , Shim- pack PRC-ODS 250 mm x 20 mm x 2, gradient: CH3CN / 10 mm/L NH4HC03, 17 min) to give the desired product (15 mg, 15% yield). ? NMR(MeOD- 4, 500 MHz): delta 8.09 (s, 1H), 7.90 (d, J = 5.5 Hz, 1H), 7.76 (s, 1H), 7.59 (m, 3H), 6.97 (d, J = 5.5 Hz, 1H). LCMS(ESI) m/z: 345.2 [M+H+].

At the same time, in my other blogs, there are other synthetic methods of this type of compound, tert-Butyl 4-amino-1H-pyrazole-1-carboxylate, and friends who are interested can also refer to it.