A gemcitabine intermediate compound

Abstract

The application belongs to the technical field of medicine synthesis, and particularly relates to a gemigim intermediate compound. The gemigim new intermediate compound is obtained by reacting 2-(1-methoxy ethylene) malonitrile and triethyl orthoformate as starting materials. Meanwhile, the application provides a method for preparing a key intermediate 3-cyano-4-methoxy-2(1H)-pyridinone of the gemigim by using the new intermediate. The synthesis method of the new intermediate is simple, the synthesis route of the gemigim prepared by using the new intermediate is short, the yield is high, the reaction condition is mild, the process is stable, and the method is suitable for mass industrial production.

Claims

1. A process for the preparation of a gemiglimine intermediate compound, characterized by, The preparation method includes the following steps: at room temperature, 12.21g of 2-(1-methoxyethylidene)malononitrile and 17.78g of triethyl orthoformate are added to 80mL of 1,4-dioxane and the reaction is carried out at 80-85℃. After the reaction is detected to be complete, the reaction solution is concentrated to dryness under reduced pressure to obtain I-1. At room temperature, 8.91 g of intermediate I-1 was added to 60 mL of 80% acetic acid solution, and the reaction was carried out under controlled reflux. After the reaction was completed, the reaction solution was cooled to 25°C to induce crystallization, and light yellow needle-like crystals precipitated out. The crystals were filtered, and the resulting filter cake was washed with water and dried to obtain the target product I. The synthesis route is as follows: ； 。

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