148870-57-9, name is 7,8-Dimethoxy-3-(3-iodopropyl)-1,3-dihydro-2H-3-benzazepin-2-one, belongs to iodides-buliding-blocks compound, is considered to be a conventional heterocyclic compound, which is widely used in drug synthesis. The chemical synthesis route is as follows. category: iodides-buliding-blocks
A mixture of (8)-N- [(4,5-dimethoxybenzocyclobut- 1 -yl)methyl] -N-(methyl)amine hydrochloride (50.36g) and dimethyl formamide (200mL) ws stirred for about 5mm andpotassium carbonate (178.46g) was added to it. The reaction mixture was stirred for about lh at about room temperature. The reaction mixture was cooled to about 5C to about 10C. 7,8-dimethoxy-3 -[3-iodopropyl]- 1,3 -dihydro-2H-3 -benzazepin-2-one (I 00g) prepared as in Example 8, was added to the stirred reaction mixture. The reaction mixture was stirred for about 6h at about 20C to about 25C. The reaction mixture was quenchedinto chilled demineralized water at about 5C to about 10C. The reaction mixture was acidified to pH of about I to about 2 using concentrated hydrochloric acid and ethyl acetate was added to it. The reaction mixture was stirred and the two layers were separated. The aqueous layer was basified to pH of about 8 to about 9.5 using 20-25% aqueous ammonia solution and ethyl acetate was added to it. The reaction mixture wasstirred and the two layers were separated. The organic layer was treated with activated charcoal, stirred at about room temperature for about 30mm, filtered over hyflo bed and washed with ethyl acetate.To the above ethyl acetate layer, was added 10% palladium charcoal (15g) and the reaction mixture was hydrogenated in an autoclave under hydrogen pressure of about8kg/cm3 to about IOkg/cm?at about 65C to about 70C for about 6h. After completion of reaction, the reaction mixture is cooled to about 20C to about 25Cand filtered overhyflo bed. The hyflo bed was washed with ethyl acetate. The reaction mixture was concentrated at about below 50C under reduced pressure and acetonitrile (400mL) and isopropyl alcohol hydrogen chloride (IPA-HCI) (3OmL) was added to it at about 5C toabout 10C. The reaction mixture was stirred at about 10C to about 15C for about 3h. The reaction mixture was concentrated at about below 50C under reduced pressure and acetonitrile (400mL) was added to it. The reaction mixture was heated to about 80C to about 85C and stirred at about the same temperature for about lh. The reaction mixture was cooled and the solid obtained was filtered, washed with acetonitrile and dried at about 50C to about 55C.Yield: 85%; 1-IPLC purity: > 98%
The synthetic route of 148870-57-9 has been constantly updated, and we look forward to future research findings.
Reference:
Patent; GLENMARK PHARMACEUTICALS LIMITED; GLENMARK GENERICS LIMITED; BHIRUD, Shekhar Bhaskar; BHUSHAN, Kumar Hari; ZOPE, Sunil Sudhakar; PATIL, Dipak Vinayak; DHEBADE, Pramod Amrutrao; CHAND, Prem; WO2014/102827; (2014); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com