Potassium Iodide → HCID 57961562, compound

Participants

Reaction Steps

To a suspension of 6-chloro-2,4,8,18,22-pentaazatetracyclo[14.3.1.1(3,7).1(9,13)]docosa-1(20),3(22),4,6,9(21),10,12,16,18-nonaen-12-amine trihydrochloride (30.0 mg, 0.067 mmol) (prepared in Example B19, step F) in 2.0 M of sulfuric acid in water (0.502 mL) was added a solution of sodium nitrite (6.93 mg, 0.10 mmol) in water dropwise at 0° C. After addition, the resultant cloudy solution was stirred at same temperature for 1 h. Then this cold solution was added dropwise to a solution of potassium iodide (16.7 mg, 0.10 mmol) and copper cyanide (0.90 mg, 0.01 mmol) in water at 0° C. The resultant mixture was stirred at rt overnight. The precipite was filtered and washed by water and dried to give the desired product as a light brown powder (28 mg, 93%). LCMS for C17H14ClIN5 (M+H)+: m/z=449.9.

Provenance & Evidence