6H-Pyrido[3',2':4,5]iMidazo[1,2-d][1,4]diazepine, 3-broMo-7,8,9,10-tetrahydro- synthesis

Yield:1239883-36-3 83%

Reaction Conditions:

with potassium carbonate in water;isopropyl alcohol at 80; for 2 h;

Steps:

329

I-109 (0.60 g, 1.37 mmol) and K₂CO₃ (0.47 g, 3.42 mmol) were dissolved in a 1:1 mixture of isopropanol and H₂O (4 mL) and the reaction mixture was stirred at 80° C. for 2 hours. The reaction mixture was concentrated and the residue was dissolved in ethyl acetate and washed with brine. The combined organic layers were dried over Na₂SO₄, the solids were filtered and the filtrate was concentrated by evaporation to give I-110 (0.30 g, 83%). MS (ESI): m/z 268 (M+1)⁺.

References:

US2010/204214,2010,A1 Location in patent:Page/Page column 119-120