Synthesis process of 1-acetyl-4-[3-(methyloxy)-4-nitrophenyl]piperazine

Abstract

The invention discloses a synthesis process of 1-acetyl-4-[3-(methyloxy)-4-nitrophenyl]piperazine, and relates to the fields related to the pharmaceutical and chemical industry. The advantages of cheap reaction raw materials, simple reaction operation, high yield and simple post-treatment are achieved through an optimized reaction process and a two-step reaction with one-step operation. The process comprises the steps that 200 grams of 1eq 5-fluorine-2-nitroanisole and 302 grams of a 3eq DMF solution of piperazine are stirred for 30 minutes, then heating is carried out for a reaction for 12 hours, 358 grams of 3eq acetic anhydride is slowly added into a reaction solution, the reaction solution is stirred for 12 hours at the room temperature, water is added into the reaction solution for dilution, after solid filtration is carried out, washing is carried out 2 times, and after drying at 50 DEG C is carried out, the product is obtained, wherein the filter liquor after filtration can be used for recycling 1-acetylpiperazine.

Description

technical field [0001] The invention relates to the related fields of medicine and chemical industry, in particular to a synthesis process of 1-acetyl-4-[3-(methyloxy)-4-nitrophenyl]piperazine. Background technique [0002] 1-acetyl-4-[3-(methyloxy)-4-nitrophenyl]piperazine English name is 1-(4-(3-methoxy-4-nitrophenyl)piperazin-1-yl)ethanone , CAS number is 1116229-11-8, molecular formula is C 13 h 17 N 3 o 4 , the molecular weight is 279.29178. [0003] There are three synthetic methods for 1-acetyl-4-[3-(methyloxy)-4-nitrophenyl]piperazine in the current literature, and the disadvantages of each synthetic method are as follows: [0004] method 1: [0005] [0006] Disadvantages: multi-step reaction operation, low reaction yield, complicated purification method; [0007] Method 2: [0008] [0009] Disadvantages: the reaction route is long, the reaction operation is complicated, multiple filtration and drying are required, the reaction yield is low, and the p...

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Problems solved by technology

[0006] Disadvantages: multi-step reaction operation, low reaction yield, complicated purification method;

[0009] Disadvantages: the reaction route is long, the reaction operation is complicated, multiple filtration and drying are required, the reaction yield is low, and the purification method is complicated;

[0012] Disadvantage: The initial reaction raw material (1-acetylpiperazine) is expensive

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