反应详情

温度

80 °C

Next, cyclohexyl-N-(1,2,2,2-tetrachloro-1-hydroxyethyl) carboxamide 4 was synthesized as follows. A mixture of compound 3 (8.0 g, 20 mmol) and thionyl chloride (4.7 mL, 63.8 mmol, 2.2 equivalents) in dry benzene (30 mL) was heated at 80° C. in an oil bath. The initial suspension eventually became a clear solution (reaction time depends on the amount of starting materials, in this example it took about 5 hours). The mixture was stirred for an additional 30 minutes. The solvents were removed by evaporation under reduced pressure (rotovapor), and the resulting white solid was washed with hexanes and filtered, to produce the desired product 4 (7.0 g). NMR (1H, CDCl3): δ 6.59 (d, 1H), 6.30 (d, 1H), 2.19 (m, 1H), 1.89-1.19 (m, 10H).

1. customNext, cyclohexyl-N-(1,2,2,2-tetrachloro-1-hydroxyethyl) carboxamide 4 was synthesized
2. customreaction time
3. customThe solvents were removed by evaporation under reduced pressure (rotovapor)
4. washthe resulting white solid was washed with hexanes
5. filtrationfiltered