Preparation method of tropisetron hydrochloride
A technology for tropisetron hydrochloride and preparation steps, which is applied in the field of preparation of tropisetron hydrochloride, can solve problems such as expensive n-butyllithium, hidden dangers in production safety, and difficulty in evaporation to dryness, and saves workload and cost. , the effect of easy operation
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[0032] (1) Preparation of (II) ( Figure 4 ):
[0033] Add reactant (I) (50g, 0.31mol) and dichloromethane (300mL) into the reaction flask, cool down to about 0°C, then add thionyl chloride (27mL, 0.37mol) dropwise to the above reaction flask During the middle, the drop was completed, raised to room temperature and stirred for 2 hours, and TLC monitored the progress. After the reaction was complete, the reaction system was concentrated to dryness at room temperature under reduced pressure to obtain a yellow solid (II), regardless of weight and yield, which was dissolved by adding tetrahydrofuran (400mL). directly used in the next step reaction;
[0034] (2) Preparation of (IV) ( Figure 5 ):
[0035] Add (Ⅲ) (43.8g, 0.31mol), tetrahydrofuran (400mL), and triethylamine (64.5mL, 0.47mol) into the reaction flask, and add the tetrahydrofuran solution of 3-indolecarbonyl chloride prepared above to the reaction flask dropwise. In the bottle, after dropping, raise the temperature...
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