288-32-4, 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. 288-32-4, name is 1H-Imidazole, A new synthetic method of this compound is introduced below.
Preparation of Imidazol-1-ylacetic acid. Into a 1-L, three-necked RB flask is charged 100g of imidazole, 40ml of DMF, 400ml of toluene, 180g of potassium carbonate and lOg of potassium iodide. After stirring for 10min, 240g of methyl chloroacetate was added slowly over a period of 1.5-2. Ohr at 25- 30C. The reaction mass was kept under stirring at 25-30 C for lhr and slowly heated to 60-65C. After maintaining at the same temperature for 2-3h reaction was found to be over by TLC. The reaction mass was cooled to 25-30C and added 200ml of ethyl acetate. The reaction mass was stirred for 20-30min and decanted the top organic layer. The residue was once again extracted with ethyl acetate (200ml). Finally water (200ml) was added to the reaction mass and stirred for 30min. Inorganic salts were removed by filtration and the filtrate extracted with ethyl acetate (2 x 200ml). All ethyl acetate extractions were combined and distilled off under vaccum to get 220g of crude mass. The crude mass was suspended in 500ml of water and refluxed for 4-5h. Reaction mass became a clear liquid. The reaction mass was treated with charcoal and distilled off water under vaccum keeping the temperature below 80C. The residue was cooled to 25-30C and added 250ml of methanol. The suspension was stirred for lh and filtered the mass. The wet cake was washed with 50ml of methanol and dried at 50-60C to get 150g of white crystalline solid of imidazol-1-ylacetic acid. Melting point is 268-269 C. Purity by HPLC is 99.2%.
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:
Patent; NATCO PHARMA LIMITED; PULLA REDDY, Muddasani; USHA RANI, Vattikuti; VENKAIAH CHOWDARY, Nannapaneni; WO2005/63717; (2005); A1;,
Imidazole – Wikipedia,
Imidazole | C3H4N2 – PubChem