1. 1 main instruments and reagents:

Model 2996/2487 high performance liquid chromatograph produced by Waters Company of the United States; 360FI-IR infrared spectrometer produced by Niccoli Company and YRF-3 melting point instrument produced by Tianjin University Precision Instrument Factory; 6890N gas chromatograph produced by Agilent Company of the United States. Adenosine (produced by Jiangsu Cheng Yi Pharmaceutical Co., Ltd., content 99.4%); Acetic anhydride, acetic acid and p-toluenesulfonic acid are all industrial grade; The reagent used for analysis is analytically pure or chromatographically pure.

1.2 experimental method:

1.2. 1 preparation of acetyladenine;

Add 250g of acetic anhydride, 7.5g of acetic acid and 50g of adenosine (0.187mol) into the reaction bottle, stir and raise the temperature to 10 ~ 120℃ for clarification, add 0.5g of p-toluenesulfonic acid and keep the temperature for 60-90min until the feed liquid becomes turbid, and then continue the reaction for 3-3. Filtering, washing the filter cake with proper amount of water, and drying to obtain light yellow solid acetyladenine about 365,438 0 g, with a yield of 94% (single impurity ≤ 0.65,438 00% (HPLC), tetra-acetylribose ≤ 0.5% (GC)).

Preparation of 1.2.2 adenine;

22.7 g of water, 1 1.8 g of sodium hydroxide and 3 1 g of acetanilide (0. 175 mol) were put into a reaction bottle, heated to 85-95℃ for clarification, decolorized and filtered with activated carbon, and the filtrate was kept at 85-95℃ for 2 hours. The infrared spectrum of the product is consistent with the standard spectrum; MP 357 ~ 359℃ (refer to [1] MP 354 ~ 358℃); Content ≥ 99.7% (HPLC); Single impurity ≤ 0. 10%(HPLC)}.

2 Results and discussion:

2. 1 There is a lot of adenosine (fermentation) in the market. Adenine is refined from adenosine by acetylation and hydrolysis, with few process steps and simple operation. The total yield is as high as 90%, which is much higher than 50% of hypoxanthine process. At the same time, the new process has high unit output of adenine and good product purity, which is suitable for industrial scale production.

2.2 The new adenosine process does not use organic solvents such as phosphorus oxychloride and pyridine, which is beneficial to environmental protection. In the reaction, acetic anhydride, acetic acid and other solvents can be recycled, and the three wastes are rarely easy to treat; At the same time, tetraacetylribose, a by-product of the reaction, is also a commonly used pharmaceutical intermediate in chemical synthesis, which can be comprehensively utilized to reduce the cost. This process is a green and environmentally friendly new process suitable for industrial production of adenine.