2 results about "Trelagliptin" patented technology

The application provides a one-pot preparation method of a key intermediate of tigilazone, and belongs to the technical field of medicine manufacturing. 5-amino-3-methyl-1-phenylpyrazole is used as raw material, nitramination and halogenation are carried out, then condensation with Boc-piperazine is carried out, and then deprotection one-pot preparation is carried out. The application not only avoids the explosive system of NaH / DMF in the traditional process, but also avoids the use of reagents such as POCl3, the reaction is mild and environment-friendly, raw materials are easy to obtain, the yield is high, and the method is suitable for industrial production.

The invention relates to the technical field of medicine component analysis, in particular to an analysis method for determining a thiazolidine impurity in tigliptin hydrobromide, which adopts gas chromatography for detection and comprises the following steps: a chromatographic column takes 5% diphenyl-1% vinylbenzene-94% dimethyl polysiloxane or substances with similar polarity as a stationary liquid; the initial temperature is 50-150 DEG C, the temperature is maintained for 5-15 minutes, then the temperature is increased to 300-360 DEG C at the speed of 10-30 DEG C per minute, and the temperature is maintained for 5-25 minutes; the temperature of a sample inlet is 280-340 DEG C; the temperature of the detector is 305-365 DEG C; the sample injection volume is 1-5 [mu] l; the flow velocity of the carrier gas is 2-5ml per minute; the split ratio is (15: 1)-(25: 1); the tetrahydrothiazole impurity has a basic toxicity warning structure, and the content of the tetrahydrothiazole impurity is directly related to the medication safety of the tigliptin hydrobromide, so that the content of the impurity in the tigliptin hydrobromide can be accurately determined, the level of the harmful impurity in the raw material medicine can be effectively monitored, the medication risk possibly caused by excessive impurity is avoided from a quality control link, and the safety of the quality control link is improved. The medication safety of patients is ensured.