反应详情

温度

80 °C

First, cyclohexyl-N-(2,2,2-trichloro-1-hydroxyethyl)carboxamide 3 was synthesized as follows. A mixture of chloral hydrate (9.0 g, 54,5 mmol) and cyclohexane carboxamide (5.0 g, 49.5 mmol) 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 6 hours). The mixture was stirred for an additional 30 minutes, then removed from the oil bath, and left at room temperature. Upon cooling, the crystalline solid formed was filtered and washed with hexanes to give the product cyclohexyl-N-(2,2,2-trichloro-1-hydroxyethyl)carboxamide 3 (11.0 g). NMR (1H, CDCl3): δ 6.23 (d, J=8.4 Hz, 1H), 5.9 (dd, 1H), 4.35 (broad s, 1H), 2.16 (t, 1H), 1.90-1.22 (m, 10H).

1. customFirst, cyclohexyl-N-(2,2,2-trichloro-1-hydroxyethyl)carboxamide 3 was synthesized
2. customreaction time
3. customremoved from the oil bath
4. waitleft at room temperature
5. temperatureUpon cooling
6. customthe crystalline solid formed
7. filtrationwas filtered
8. washwashed with hexanes