反应详情

A solution of 4-(2-ethyl-1-(1H-imidazol-1-yl)butyl)aniline (285 mg, 1.17 mmol) and KSCN (455 rug, 4.68 mmol) in AcOH (6 mL) was stirred until all dissolved at RT and then treated with Br2 (0.063 mL, 1.23 mmol) in AcOH (2 mL) added drop wise via syringe over 5 min. The reaction mixture was stirred overnight at RT. The reaction mixture was diluted with ice water and then basified with NH4OH (pH 12). The aqueous phase was extracted three times with DCM and the organic extracts were combined and dried over filtered and then concentrated. The crude product was purified by preparative TLC using 5% MeOH in DCM as eluent to afford to 6-(2-ethyl-1-(1H-imidazol-1-yl)butyl)benzo[d]thiazol-2-amine as pale yellow solid. MS (ES+): 301.27 (MH+).

1. dissolutionall dissolved at RT
2. additionadded drop wise via syringe over 5 min
3. extractionThe aqueous phase was extracted three times with DCM
4. customdried
5. filtrationover filtered
6. concentrationconcentrated
7. customThe crude product was purified by preparative TLC