反应详情

1,3-dichloroacetone (0.01 mL, 0.11 mmol) was added dropwise to a solution of 6-trifluoromethyl-pyridin-2-ylamine (0.016 g, 0.10 mmol) in 1,2-dimethoxyethane (1.0 mL), and the mixture was left to stir at room temperature for 2 h. The solvent was removed in vacuo and the resulting residue re-dissolved in ethanol (1.0 mL). The reaction mixture was subsequently heated under reflux for 2 h, and the solvent was removed under reduced pressure. DIPEA (0.05 mL, 0.25 mmol) and 1-methyl-4 phenyl-1,3-dihydro-imidazole-2-thione (0.017 g, 0.09 mmol) were sequentially added to a solution of the crude product in DMF (1.0 mL). The reaction mixture was then heated at 60° C. for 2 h after which LC-MS showed complete consumption of the starting materials. The solvent was removed under reduced pressure and the crude product purified using preparative LC-MS to yield the title compound. LC-MS: m/z=389.1 (MH+), tR=0.52 min, method C.

1. waitthe mixture was left
2. customThe solvent was removed in vacuo
3. dissolutionthe resulting residue re-dissolved in ethanol (1.0 mL)
4. temperatureThe reaction mixture was subsequently heated
5. temperatureunder reflux for 2 h
6. customthe solvent was removed under reduced pressure
7. temperatureThe reaction mixture was then heated at 60° C. for 2 h after which LC-MS
8. customconsumption of the starting materials
9. customThe solvent was removed under reduced pressure
10. customthe crude product purified