Tag: M.W:100-200

Electric Literature of 82560-12-1,Some common heterocyclic compound, 82560-12-1, name is 3-Amino-5-tert-butylpyrazole, molecular formula is C7H13N3, 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 2,4-dichloropyrimidine (3.73g, 25mmol) and 5-amino-3-tert-butyl-lH- pyrazole (3.55g, 25.5mmol) and DIPEA (4.44ml, 25mmol) were heated at 5O0C in TEtaF25 (75ml) for 18 hours under nitrogen. The mixture was allowed to cool and the volatiles removed by evaporation. The residue was dissolved in DCM (150ml), washed with water, dried (MgSO4) and the solvent removed by evaporation. The residue was purified by chromatography on silica gel eluting with EtOAc/hexanes (1:3) and then methanol/DCM (5:95) to give 2-chloro-4-(5-tert-butyl-lH-rhoyrazol-3-ylamino)rhoyrimidine (1.73g, 28%). NMR30 Spectrum 1.30 (s, 9Eta), 6.05 (s, IH), 7.16 (br s, IH), 8.12 (d, IH), 9.80 (br s, IH), 11.89 (br s, IH); Mass Spectrum 252 [MH]+.

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-tert-butylpyrazole, 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. 3398-16-1, name is 4-Bromo-3,5-dimethylpyrazole, A new synthetic method of this compound is introduced below., SDS of cas: 3398-16-1

with reflux condenser and magnetic force to the rotor of the dry three-mouth bottle is sequentially added in the 3, 5 – dimethyl -4 – brompyrazole (5250 mg, 30 . 00 mmol, 1 . 00 equivalent), cuprous iodide (572 mg, 3 . 00 mmol, 0 . 10 equivalent), L – proline (690 mg, 6 . 00 mmol, 0 . 20 equivalent), potassium carbonate (8280 mg, 60 . 00 mmol, 2 . 00 equivalent) replacing nitrogen three times, then adding iodine anisole (10500 mg, 45 . 00 mmol, 1 . 50 equivalent) and steams again dimethyl sulfoxide (10 ml). The reaction mixture to the 120 C under stirring 2 days, TLC thin layer chromatographic monitoring until the raw material 4 – brompyrazole reaction finishes. The addition of water (100 ml) quenching the reaction, filtration, 50 ml ethyl acetate full washing insolubles, separating the mother liquor in the organic phase, dried with anhydrous sodium sulfate, filtered, the solvent removed by reduced pressure distillation. The obtained crude product through the silica gel column chromatography separation and purification, eluent (petroleum ether/ethyl acetate=20:1 – 10:1), to obtain compound 1 colorless viscous liquid 8350 mg, yield 99%.

The synthetic route of 3398-16-1 has been constantly updated, and we look forward to future research findings.

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. 3524-32-1, name is 5-Amino-1,3-dimethylpyrazole, This compound has unique chemical properties. The synthetic route is as follows., Application In Synthesis of 5-Amino-1,3-dimethylpyrazole

General procedure: A mixture of salicylaldehydes 1 (1 mmol), 4-hydroxy-6-methyl-2H-pyran-2-one 2 (1mmol) and L-proline (0.10 mmol) in EtOH (10 mL) was stirred at 80 C for 1 h. Then pyrazol-5-amines 3(1 mmol) and CuSO4 (0.20 mmol) was added to the reactor and stirred at 80 C for 4-48 h. Aftercompletion of the reaction confirmed by TLC (eluent acetone/petroleum ether (PE), V/V = 1:3), thereaction mixture was concentrated in vacuo to remove the solvent. The product purified by columnchromatography (PE-acetone = 5:1) to afford the pure product 4.

According to the analysis of related databases, 3524-32-1, 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.

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.

Adding a certain compound to certain chemical reactions, such as: 175137-46-9, name is 5-Cyclopropyl-1H-pyrazol-3-amine, 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 175137-46-9, category: pyrazoles-derivatives

A solution of 2,4,5-trichloropyrimidine (533 mg, 2.93 mmol), 3-amino-5-cyclopropyl- lH-pyrazole (360 mg, 2.93 mmol) and triethylamine (0.49 ml) in EtOH (5 ml) was stirred at room temperature for 10 hours. Solvent was removed and EtOAc was added. The solution was washed with water and dried over anhydrous sodium sulfate and was concentrated to give title compound as a white solid (546 mg, 69%). The compound was carried to the next step without further purification. 1HNMR delta 0.92 (m, 2H), 1.20 (m, 2H), 2.18 (m, IH), 6.40 (s, IH), 8.60 (s, IH), 9.90 (s, IH), 12.60 (s, IH).

If you are interested in these compounds, you can also browse my other articles.Thank you for taking the time to read this article. I hope you enjoyed it.

Related Products of 3112-31-0, A common heterocyclic compound, 3112-31-0, name is 1H-Pyrazole-3,5-dicarboxylic acid, molecular formula is C5H4N2O4, 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.

In a typical synthesis, 0.17mmol (0.0300g) of H3dpc, 0.36mmol (0.0586g) of MnCl2 2H2O, 0.26mmol (0.0403g) of 4,4?-bpy and 10mL of distilled water were mixed. The reaction mixture was stirred until a homogeneous gel was formed (pH 4), sealed in a PTFE-lined stainless steel autoclave with an internal volume of 40mL and heated at 150¡ãC for 3days under autogenous pressure. After cooling to room temperature, the resulting block single crystal particles that was confirmed to be compound 3 by XRD were filtered off, washed with distilled water (3*50mL), and dried in an ambient condition. Yield 0.031g, 73percent based on H3dpc. The mother liquor was allowed to stand still for evaporation. After one week, small amount single crystals were found grown up on the wall of beaker. These crystal particles were collected and air dried at room temperature, single crystal X-ray diffraction data revealed that these particles were phase 1. Yield 0.010g, 9.4percent based on H3dpc.

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 52222-73-8, The chemical industry reduces the impact on the environment during synthesis 52222-73-8, name is 4-(Trifluoromethyl)-1H-pyrazole, I believe this compound will play a more active role in future production and life.

To a solution of 2-chloro-5-nitrobenzonitrile (1 .278 g, 7.0 mmol) and 4-(trifluoromethyl)- iH-pyrazole (1 .0 g, 7.35 mmol) in acetonitrile (10 mL) was added potassium carbonate (2.90 g, 21 mmol) at RT. The mixture was heated to 60 C and stirred at this temperature for 1 hour. The reaction mixture was diluted with EtOAc (50 mL), and the solids were removed by filtration. The filtrate was concentrated in vacuo and the residue was purified by Biotage Isolera chromatography (silica gel, eluting with heptanes-EtOAc, 1 :0 to 0: 1 ). The product containing fractions were combined and concentrated in vacuo to afford 1 .77 g (89% yield) of the title compound as a yellow solid.1H NMR (500 MHz, DMSO-d6) delta [ppm] 9.28 (s, 1 H), 8.94 (d, J = 2.6 Hz, 1 H), 8.68 (dd, J = 9.0, 2.6 Hz, 1 H), 8.47 (s, 1 H), 8.19 (d, J = 9.0 Hz, 1 H).LCMS (Analytical Method A): Rt = 1 .16 mins; MS (ESIpos) m/z = 283.0 (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, 4-(Trifluoromethyl)-1H-pyrazole, other downstream synthetic routes, hurry up and to see.

Electric Literature of 66121-71-9, The chemical industry reduces the impact on the environment during synthesis 66121-71-9, name is 4-Cyano-1-methylpyrazole, I believe this compound will play a more active role in future production and life.

1-Methyl-1H-pyrazole-4-carbonitrile (18 gm, 0.168 moles) obtained in step 2, tn-nbutyl tin chloride (65 gm, 0.2 18 moles), sodium azide (14 gm, 0.20lmoles) were taken in toluene (180 ml). The reaction mixture.was stirred for 24 hours at 100-120C. The progress of the reaction was monitored by HPLC. The above reaction mixture was cooled to 10- 15C, to this added 10% ethanolic HCI solution (100 ml, pH= 1-2). The reaction mixturewas stirred for 1-1.5 hours at 10-15C, filtered off the inorganic salts, washed with ethanol (30 ml). The mother liquor and washings were collected and toluene and ethanol were recovered at 50-55C at reduced pressure. To the above residue at 20-25C, added diisopropyl ether (100 ml), stirred for 1-2 hours at 20-25C, filtered the solid, washed with diisopropyl ether (30 ml) and air dried the product, 5-(1-methyl-IH-pyrazol-4-yl)-2H-tetrazole at 60-65C.Drywt25gm1.4 w/w (99%)1.40w/wYieldTheoretical yield

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

Reference of 5203-77-0,Some common heterocyclic compound, 5203-77-0, name is 1,3-Dimethyl-1H-pyrazol-5-ol, molecular formula is C5H8N2O, 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: Intermediate 7 (4mmol), dissolved in dry dichloromethane (60mL), and PCl5 (4.2mmol) were added and stirred at room temperature for 1h. The solvent was moved out under reduced pressure to afford acid chloride, the acid chloride was then dissolved in dry CH2Cl2 (60mL), Then 1-methyl-1H-pyrazol-5-ol (4mmol) and Et3N (4.8mmol) were added to the above solution, and stirred for a further 18-24hat room temperature. After adding dichloromethane (30mL), the resultant mixture was washed sequentially with 2N hydrochloric acid (100mL), saturated NaHCO3 and saturated NaCl and dried over Na2SO4. The rest of the solution was evaporated in vacuum and purified by silica gel column chromatography using gradient elution of ethyl acetate/hexane (V:V = 1:2) to obtain the desired intermediate 8 as a write powder (30%-70%). 4.1.10 1-methyl-1H-pyrazol-5-yl3-methyl-2-oxo-1-propyl-2,3-dihydro-1H-benzo[d] imidazole- 5-carboxylate Yield: 45%. m.p. 107-108C. 1H NMR (600MHz, CDCl3) delta 8.01 (dd, J=8.4, 1.2Hz, 1H), 7.77 (d, J=1.2Hz, 1H), 7.48 (d, J=1.8Hz, 1H), 7.10 (d, J=8.4Hz, 1H), 6.20 (d, J=1.8Hz, 1H), 3.92 (t, J=7.2Hz, 2H), 3.80 (s, 3H), 3.51 (s, 3H), 1.91-1.71 (m, 2H), 1.00 (t, J=7.8Hz, 3H). EI-MS (m/z): 314.18 (M)+.

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