反应详情

温度

-78 °C

2,5-Dibromo-4-methylpyridine (1.83 g, 7.29 mmol) was dissolved in toluene (100 mL), cooled to −78° C. and a solution of nBuLi (4.4 mL, 8.8 mmol, 2.0 M in pentane) was added dropwise and stirred at −78° C. for 2 h. A solution of tBuNCO (1.1 mL, 9.5 mmol) in toluene (3 mL) was added dropwise and stirred for 1 h at −78° C. then warmed to −10° C. and quenched by addition of NH4Cl (aq). After warming to r.t. the reaction was extracted with ether and the organics dried over Na2SO4 and concentrated. The product was used without further purification. MS [M+H]+: 271.0; tR=2.44 min. (method 1)

1. stirringstirred for 1 h at −78° C.
2. temperaturethen warmed to −10° C.
3. customquenched by addition of NH4Cl (aq)
4. temperatureAfter warming to r.t. the reaction
5. extractionwas extracted with ether
6. dry with materialthe organics dried over Na2SO4
7. concentrationconcentrated
8. customThe product was used without further purification