These common heterocyclic compound, 39806-90-1, name is 4-Iodo-1-methyl-1H-pyrazole, 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. name: 4-Iodo-1-methyl-1H-pyrazole
Step 2: l -methyl-l H-pyrazole-4-carbonitrile To a solution of 4-iodo- l -methyl- 1 H-pyrazole (55 gm, 0.264 moles) in N,N- dimethylacetamide ( 100 ml) was added potassium ferrocyanide (24.5 gm, 0.058 moles), palladium (II) acetate (0.592 gm, 0.0026 moles) and sodium carbonate (27.98 gm, 0.264 ,moles). The reaction mixture was evacuated and backfilled with nitrogen (3 times). The mixture was stirred for 12 hour at 90- 1 10C. Progress of the reaction was monitored by HPLC. The reaction mixture was cooled to 20-30C, to this added DI water (500 ml), ethyl acetate (500 ml) and stirred for 1 hour at 20-30 C. The reaction mixture was filtered through pad of celite. The organic layer was separated and aqueous layer was extracted with ethyl acetate (200 ml), stirred for 15 min and separated the final aqueous layer and organic layer. The organic layer was washed with brine solution (200 ml). Ethyl acetate was recovered at reduced pressure at 60-70C. The mixture was degassed for 2 hour at reduced pressure at 60- 70C, cooled the mixture to 20-30C. Hexane (400 ml) was added to the mixture and stirred for 1 hour at 20-30C. The solid product obtained was filtered off, washed with cold DI water (100 ml) and dried at 40-50 C to yield the product, 1 -methyl- l H-pyrazole-4-carbonitrile,. Dry wt : 17.94 gm Yield : 0.32 w/w (63%);
The synthetic route of 4-Iodo-1-methyl-1H-pyrazole has been constantly updated, and we look forward to future research findings.