反应详情

(See, e.g., Tsupak et al., Khimiya Geterotsiklicheskikh Soedinenii. 7:1096-1102 (2003); Tsupak et al., Russ. Chem. Bull. 55:2265-2270 (2006)). To a solution of 3 (2.61 g, 10.1 mmol) in chloroform (13 mL) was added bromine (1.62 g, 0.52 mL, 20.3 mmol in 3 mL chloroform) dropwise over 30 min at room temperature. The reaction mixture was further stirred for 1 min at room temperature before concentrated in vacuo. The crude reaction mixture was purified by flash chromatography to yield 4 (1.96 g, 57%); mp 164-167° C.; MS (ES+) (m/z): [M+1]+ calculated for C14H14BrN2O3, 338.18. found 337.15, 338.93. This compound matched analytical data as reported (see, e.g., Tsupak et al., Khimiya Geterotsiklicheskikh Soedinenii., supra; Tsupak et al., Russ. Chem. Bull., supra).

1. concentrationbefore concentrated in vacuo
2. customThe crude reaction mixture
3. customwas purified by flash chromatography