反应详情

IV (7.5 g, 0.018 mole) and absolute ethanol (300 ml) were placed in a flask and warmed slightly to dissolve all of the crystals. Then the solution was saturated with anhydrous ammonia while the flask was cooled in ice water. White needles separated after the clear solution stood at room temperature for 3 days. The mixture was cooled in ice water, and the crystals were filtered and washed with a small amount of cold ethanol. A second crop of crystals, 1.1 g, was obtained by evaporating the filtrate to a volume of 35 ml and cooling in ice water. The total yield was 6.1 g (89%), mp 185°-185.5° C. Anal. calcd. for C8H7Br3N2O: C, 24.84; H, 1.82; Br, 61.96; N, 7.24. Found: C, 24.83; H, 1.87; Br, 61.82; N, 7.26.

1. temperaturewarmed slightly
2. dissolutionto dissolve all of the crystals
3. customWhite needles separated after the clear solution
4. temperatureThe mixture was cooled in ice water
5. filtrationthe crystals were filtered
6. washwashed with a small amount of cold ethanol
7. customA second crop of crystals, 1.1 g, was obtained
8. customby evaporating the filtrate to a volume of 35 ml
9. temperaturecooling in ice water