Category: 113402-89-4

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. 113402-89-4, name is 3-Methyl-1H-pyrazol-5-amine, A new synthetic method of this compound is introduced below., HPLC of Formula: C4H7N3

4-Bromo-6,7-dimethoxycinnoline (530 mg, 2.0 mmol), 5-methyl-4H-pyrazol-3-amine (150 mg, 1.5 mmol), toluene (4 mL), tris(dibenzylideneacetone)dipalladium(0) (45 mg, 0.049 mmol), 9,9-dimethyl-4,5-bis(diphenylphosphino)xanthane (70.0 mg, 0.121 mmol) and sodium tert-butoxide (1.80E2 mg, 1.87 mmol) were combined in a 10 mL sealed tube. The reaction was irradiated in a microwave on 300 watts, at 140°C for 600 seconds The reaction mixture was then filtered through Celite using methanol and methylene chloride and subsequently concentrated. The crude product was then dissolved in 1 mL methanol and filtered through a Gelman Acrodisk 0.45 micron HPLC filter. Purification using a C18 column preparative (30 x 00 mm) HPLC column and a gradient of 20-80percent acetonitrile:water (with 0.1percent formic acid) and a flow rate of 45 mL/min afforded 40.9mg (8percent) of 6,7-dimethoxy-N-(5-methyl-4H-pyrazol-3-yl)cinnolin-4-amine hydroformate as a yellow solid. MS [M+H] = 286.1, LC/MS (EI) tR 3.14 min (Method B), .H NMR (DMS0-d6) 8 (ppm) d 12.57 (s, 1 H), 9.38 (s, 1 H), 7.94 (s, 1 H), 6.12 (s, 1.5 H), 5.75 (s, 0.5 H), 4.01 (s, 3 H), 4.00 (s, 3 H), 2.30 (s, 3 H)

The synthetic route of 113402-89-4 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; MEMORY PHARMACEUTICALS CORPORATION; WO2006/28957; (2006); A1;,
Pyrazole – Wikipedia,
Pyrazoles – an overview | ScienceDirect Topics

Related Products of 113402-89-4, 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 113402-89-4 as follows.

Will 10mmol compound 1,10 mmol of compound 2 and 1 mmol of K2CO3 and 10 mL of PEG 400 were added to the reaction flask.Reaction at 80 ° C for 24 h,The reaction solution was cooled to room temperature.Precipitating in ether,The filtrate was collected by filtration.Purified by gel chromatography (mobile phase petroleum ether / ethyl acetate = 5:1),Compound 3;Compound 3 (1 mmol),Raney Nickel (0.1g),Sodium n-propoxide (0.92 g, 11 mmol) was dissolved in 50 mL of 1,2-dimethoxyethane.Reaction at 60 ° C for 10 h,Cool to room temperature,Collect organic phase by filtration,Removal of 1,2-dimethoxyethane by rotary evaporation,The compound 62 was purified by column chromatography using acetonitrile / dichloromethane (5:1 by volume).

According to the analysis of related databases, 113402-89-4, the application of this compound in the production field has become more and more popular.