反应详情

A solution of 100 mg (0.30 mmol) of 8-chloro-1-(2-chloro-phenyl)-1H-imidazo[4,5-c]quinoline 5-oxide (Example 71), 50 μl dry DMF, and 86 μl POCl3 in 2 ml toluene is stirred at 70° C. bath temperature for 3½ h. First, ice is added to the cold reaction mixture, then water and ethyl acetate. The phases are separated and the water phase is extracted with ethyl acetate. The combined organic phases are washed with water and brine, then dried over Na2SO4. After the solvent is evaporated, the residue is crystallized from ethyl acetate-hexane. mp: 194-200° C.; MS: 348 (M++1); HPLC: tret=13.54 min (Grad 1).

1. additionFirst, ice is added to the cold reaction mixture
2. customThe phases are separated
3. extractionthe water phase is extracted with ethyl acetate
4. washThe combined organic phases are washed with water and brine
5. dry with materialdried over Na2SO4
6. customAfter the solvent is evaporated
7. customthe residue is crystallized from ethyl acetate-hexane
8. customtret=13.54 min (Grad 1)