反应详情

温度

0 °C

To a solution of 8-iodo-6-{[4-(trifluoromethoxy)phenyl]sulfonyl}-2-(trifluoromethyl)-6,11-dihydro-5H-pyrido[2,3-b][1,5]benzodiazepine (380 mg, 0.618 mmol, intermediate 61) in 2 ml of THF was added a solution of isopropyl magnesium chloride (1.54 ml, 3.08 mmol) in THF (2M) at 0° C. and the solution was stirred for 30 min at 0° C. Then the reaction mixture was added to a solution of ethyl cyanidocarbonate in 3 mL of THF and stirred for 30 min at 0° C. The reaction mixture was poured into 2 mL of 2N HCl and 5 mL of ice-water, and the pH was adjusted to 7-8 with aqueous NaHCO3 at 0° C. The solution was extracted with ethyl acetate (3×20 ml), and the combined organic extracts were dried over Na2SO4. The solution was concentrated under reduced pressure and the residue was purified by silica gel chromatography using with hexane/ethyl acetate (6/1) to give the title compound as a white solid; Mass Spectrum: m/e=562 (M+1).

1. stirringstirred for 30 min at 0° C
2. extractionThe solution was extracted with ethyl acetate (3×20 ml)
3. dry with materialthe combined organic extracts were dried over Na2SO4
4. concentrationThe solution was concentrated under reduced pressure
5. customthe residue was purified by silica gel chromatography