The invention relates to the technical field of compound preparation, in particular to a preparation method of a compound N-nitrosoperindopril. The method specifically comprises the following steps: S1, selecting a first chemical which is prepared from an initial
raw material and has the HPLC detection purity of more than or equal to 99.0%, dissolving the first chemical in water, stirring, dissolving, and cooling to obtain a first mixture; s2, adding acid into the first solution to obtain a second mixture; s3,
nitrite is added into the second mixture in batches and stirred, white solids are separated out after dissolving clarification, and a third mixture is obtained; s4, after the interior of the third mixture is completely reacted, multiple times of extraction is conducted through
dichloromethane,
drying and concentration are conducted, and the off-white
solid N-nitrosoperindopril is obtained.According to the preparation method of the compound N-nitrosoperindopril, the blank that no standard substance is sold in the market and no literature is used for synthesis report is filled, and the preparation method is suitable for large-scale popularization and application of the compound N-nitrosoperindopril. And help is provided for ensuring that the safety and the quality of
medicine products are not influenced.