反应详情

A mixture of 2-n-butyl-3-[(2′-cyanobiphenyl-4-yl)methyl]-1,3-diazaspiro-[4,4]-non-1-en-4-one (10 g), sodium azide (7.7 g) and piperazine dihydrochloride (7.5 g) in xylene (30 ml) was refluxed for 7 hours under stirring. The reaction was cooled to room temperature and extracted with 5% NaOH solution. The pooled alkaline solution was washed with toluene or xylene (15 ml) and the aqueous phase neutralized to pH 6.5 using concentrated HCL. The resulting suspension was stirred for 3 hours at room temperature and filtered obtain irbesartan (3.6 g, 96% purity by HPLC).

1. temperaturewas refluxed for 7 hours
2. extractionextracted with 5% NaOH solution
3. washThe pooled alkaline solution was washed with toluene or xylene (15 ml)
4. concentrationusing concentrated HCL
5. stirringThe resulting suspension was stirred for 3 hours at room temperature
6. filtrationfiltered