Preparation method of ketone drug intermediate
A technology for intermediates and drugs is applied in the field of preparation of ketone drug intermediates, which can solve the problems that the reaction process is not meaningful for reference, and achieve the effects of simple preparation process, high yield and purity.
- Summary
- Abstract
- Description
- Claims
- Application Information
AI Technical Summary
Problems solved by technology
Method used
Image
Examples
Embodiment 1
[0014] A preparation method of a ketone drug intermediate, the ketone drug intermediate is 1-isopropyl-4,6-dihydrospiro[indazole-5,4'-piperidine]-7(1H)- Ketones, the steps of which include:
[0015] 250 g of tert-butyl 9-oxo-3-azaspiro[5.5]undec-7-ene-3-carboxylate and 325 ml of tris(dimethylaminomethane) were dissolved in 1.9 liters of toluene and heated under reflux 4 hours. The mixture was distilled and concentrated to a minimum stirred volume at 110° C., then 1.9 liters of toluene were added. The reaction was redistilled to a minimum stirred volume and cooled to room temperature. 1.8 liters of toluene and 135 grams of prohydrazine hydrochloride were added and the solution was heated to reflux for 5 hours. The reaction was cooled to room temperature and then washed with 150 mL of 10% aqueous citric acid and 200 mL of water, and the organic layer was then distilled to a minimum stirring volume. 2 liters of methanol were added and distilled to a minimum stirred volume. T...
PUM
Login to View More Abstract
Description
Claims
Application Information
Login to View More 