1-carboxy alkyl-4-nitroimidazole preparation method and application thereof
A technology of nitroimidazole and carboxyalkyl, applied in the field of biochemical industry, can solve the problems of expensive equipment, time-consuming, troublesome processing, etc., and achieve the effects of simple and effective synthesis steps and high purity of products after identification
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[0020] (1) Preparation of methyl 6-bromohexanoate: Add 1.95 g of 6-bromohexanoic acid (10 mmol) into 10 mL of methanol, slowly add thionyl chloride (15 mmol) dropwise under stirring in an ice bath, and then raise the temperature to reflux , Keep reflux for 2-3h. After the reaction was completed, spin-dry by vacuum rotary evaporation, then add methanol to spin-dry and repeat twice (10 mL / time, 2 times) to obtain the compound 6-bromohexanoic acid methyl ester, which is set aside.
[0021] (2) Preparation of 2-methyl-4-nitro-1-(6-carboxyhexyl)imidazole ester: 1.27 g of 2-methyl-5-nitroimidazole (10 mmol) was dissolved in 10 mL of N,N- In dimethylformamide (DMF), add sodium hydride (60% content, 480 mg, 12 mmol) under ice bath, stir for 10 min, remove the ice bath, return to room temperature and stir for 1 h, add methyl 6-bromohexanoate (10 mmol, dissolved in 2 mL DMF), stirred overnight at room temperature, and quenched with saturated ammonium chloride. Extracted twice with dich
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