反应详情

A 33% w/v solution of methylamine in ethanol (5.7 ml) was added dropwise to a stirred solution of 2-(5-bromopyrid-3-yl)-2-methylthiothiocarbonylcyclohexanone (1.33 g, 3.86 mmol) in ethanol (25 ml) and dichloromethane (25 ml) at 0°-5° C. The solution was stirred at room temperature for 5 hours and concentrated in vacuo at 30°-35° C. The residue was purified by flash chromatography over silica gel eluting with ethyl acetate: hexane 4:6 to give (±)-N-methyl-2-oxo-1-(5-bromopyrid-3-yl) -cyclohexanecarbothioamide (0.57 g) m.p. 201°-3° C. NMR(CDCl3) 1.68-2.16(m,4H); 2.46-2.6(m,2H); 2.66-2.8(m,2H); 3.17-3.17-3.19 (d,3H); 7.74-7.78(dd,1H); 8.38-8.39(d,1H), 8.58-8.59(d,1H); 8.8-9.0(broad singlet). Calculated for 47.7%; H,4.6%; N,8.6%. Found C, 48.2%; H,4.7%; N,8.5%.

1. concentrationconcentrated in vacuo at 30°-35° C
2. customThe residue was purified by flash chromatography over silica gel eluting with ethyl acetate: hexane 4:6