反应详情

Sodium (3.22 g) was dissolved in absolute ethanol (100 ml) and added dropwise to a suspension of 5-bromo-2-chloro-3-nitropyridine (30.2 g) in ethanol (100 ml) at 0° C. over 10 mins. The cold bath was removed and the reaction stirred at RT for 18 h. The reaction was evaporated to approximately half its volume then diluted with saturated ammonium chloride (aq) (600 ml). The reaction was stirred at RT overnight then the solids were filtered and rinsed well with water. The solids were dissolved in hot ethanol (100 ml) then diluted with hot water (500 ml) and stirred with cooling to RT for 2 hr. The solids were collected and rinsed well with water then suction dried and vacuum dried to give the title compound (26.4 g) as a dark brown solid.

1. customThe cold bath was removed
2. customThe reaction was evaporated to approximately half its volume
3. additionthen diluted with saturated ammonium chloride (aq) (600 ml)
4. stirringThe reaction was stirred at RT overnight
5. filtrationthe solids were filtered
6. washrinsed well with water
7. dissolutionThe solids were dissolved in hot ethanol (100 ml)
8. additionthen diluted with hot water (500 ml)
9. stirringstirred
10. temperaturewith cooling to RT for 2 hr
11. customThe solids were collected
12. washrinsed well with water
13. customsuction dried
14. customvacuum dried