反应详情

At 0° C., concentrated HCl was added dropwise to Me2NH (40% in water, 5.57 mL, 1.1 equiv) to acidify the amine. After the addition, 1-(2-chlorophenyl)ethanone (6.18 g, 0.04 mol) and paraformaldehyde (1.68 g, 1.4 equiv) were added. The mixture was dissolved in ethanol (20 mL) and heated to reflux for 30 h. LC-MS found the starting material was gone. The reaction mixture was cooled to rt. The volatiles were removed in vacuo. EtOAc (30 mL) was added and the suspension was stirred for 15 min. The solid was collected by filtration and washed with EtOAc (2×5 mL). The white solid was dried under vacuum to afford 1-(2-chlorophenyl)-3-(dimethylamino)propan-1-one HCl salt (5.17 g, 61% yield). LC-MS (3 min) tR=0.72 min, m/z 212, 214(M+1).

1. additionwere added
2. temperatureheated
3. temperatureto reflux for 30 h
4. customThe volatiles were removed in vacuo
5. additionEtOAc (30 mL) was added
6. filtrationThe solid was collected by filtration
7. washwashed with EtOAc (2×5 mL)
8. customThe white solid was dried under vacuum