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 3034-41-1 as follows. name: 1-Methyl-4-nitroimidazole
To the suspension of 1-methyl-4-nitro-1H-imidazole (128 mg, 1.012 mmol) in ethanol (5 mL) 5% palladium on carbon (10 mg, 0.053 mmol) was added. The reaction mixture was degassed under reduced pressure and stirred under hydrogen atmosphere at roomtemperature for 3 hours. The reaction mixture was filtered over celite layer and washed with ethanol. The filtrate was concentrated under reduced pressure, dissolved in toluene, transferred to a Schlenk flask and again concentrated under reduced pressure. 4-(5-Chloro- 3 -(4-chloro-2-fluorobenzyl)-2-methylpyrazolo [1, 5-a]pirymidyn-7-yl)morpholine obtained in Example 1, Step F (200 mg, 0.506 mmol), tris(dibenzylideneacetone)dipalladium(0)(23.2 mg, 0.025 mmol), 9,9-dimethyl-4,5-bis(diphenylphosphine)xanthene (29,3 mg, 0,05 1 mmol) and sodium carbonate (107 mg, 1.012 mmol) were added and the mixture was degassed under reduced pressure. Under argon atmosphere degassed toluene (5 mL) was added and the mixture was purged with argon for 15 minutes. Reaction mixture was heated to 100 C for 24 hours. The mixture was cooled to room temperature, diluted with ethylacetate (10 mL), filtered through celite layer and washed with ethyl acetate (25 mL). The filtrate was concentrated under reduced pressure. The residue was purified by column chromatography (silicagel, eluent: AcOEt 100% to AcOEt:methanol = 9:1, v/v). The product was hot-crystallized from AcOEt:heptan to obtain white crystals with a yield of 27% (63 mg, 0.138 mmol).
According to the analysis of related databases, 3034-41-1, the application of this compound in the production field has become more and more popular.
Reference:
Patent; CELON PHARMA S.A.; MROCZKIEWICZ, Michal; LIPNER, Joanna; GUNERKA, Pawel; DUBIEL, Krzysztof; WIECZOREK, Maciej; ZDZALIK, Daria; STANCZAK, Aleksandra; LAMPARSKA-PRZYBYSZ, Monika; STYPIK, Bartosz; WO2015/118434; (2015); A1;,
Imidazole – Wikipedia,
Imidazole | C3H4N2 – PubChem