1H-[1,4]Diazepino[1,7-a]benziMidazole, 8-broMo-2,3,4,5-tetrahydro- synthesis

Yield:1239879-65-2 95%

Reaction Conditions:

with potassium carbonate;isopropyl alcohol in water; for 2 h;Reflux;

Steps:

251

I-15 (6.5 g, 14.8 mmol) was dissolved in an aqueous solution containing 20% 2-propanol (200 mL) and solid K₂CO₃ (6.1 g, 3 eq). The reaction mixture was refluxed for 2 hours and the reaction mixture was concentrated. The residue was dissolved in water, extracted with dichloromethane, the combined organic layers were dried over sodium sulfate, the solids were removed by filtration and the filtrated was concentrated to give I-16 as a pale yellow solid (3.7 g, 95%). MS (ESI): m/z 267 (M+H⁺).

References:

US2010/204214,2010,A1 Location in patent:Page/Page column 100-101