Electric Literature of 714273-83-3, A common heterocyclic compound, 714273-83-3, name is 5-(tert-Butyl)-1H-imidazole-4-carbaldehyde, molecular formula is C8H12N2O, 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.
1 g (6.5 mmol)5- (tert-Butyl) -1H-imidazole-4-carbaldehyde was added to 7 mL DMF followed by 2.59 g (13 mmol)N, N-diacetylpiperazine-2,5-dione nitrogen protection row of the third gas,3.19g (9.8mmol) of cesium carbonate was added and the atmosphere was purged with nitrogen for three times. The mixture was stirred for 20h at room temperature without light.The reaction mixture was poured into (100 mL) ice-water, suction filtered, the filter cake was washed with water (100mL * 2), petroleum ether:Ethyl acetate = 8: 1 (90 mL). The filter cake was ultrasonically dispersed with ethanol and methylene chloride. The insoluble material was filtered off and concentrated under reduced pressure. Absolute ethanol was taken in water.Further beating with ethyl acetate (50 mL).0.89g of a tan solid was obtained(Z) -1 -acetyl-3 – ((5- (tert-butyl) -1H-imidazol-4-yl) methylene) piperazine-2,5-dione in 46% yield.
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; Tsingtao Ocean Bio-pharmaceutical Institute Co., Ltd.; Li Wenbao; Wang Shixiao; Ding Zhongpeng; Hou Yingwei; Guan Huashi; (21 pag.)CN107011331; (2017); A;,
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