反应详情

3-Quinolin-5-yl-butane-1,2-diamine (Intermediate E3) (1.8 g, 8.35 mmol) in CH2Cl2 (20 mL) was treated with a solution of 1,1′-thiocarbonyldiimidazole (1.52 g, 8.54 mmol) in CH2Cl2 (40 mL) at 0° C. for 1 h. The mixture was diluted with chloroform (40 mL) and water (60 mL). The aqueous layer was extracted with chloroform (3×30 mL) and CH2Cl2 (6×30 mL). The organic solution was dried over MgSO4, filtered and evaporated to give a residue. The material was purified by chromatography on SiO2 with 3% NH3-MeOH:CH2Cl2 to give 4-(1-quinolin-5-yl-ethyl)-imidazolidine-2-thione (Intermediate E4) 2 g (93%).

1. extractionThe aqueous layer was extracted with chloroform (3×30 mL) and CH2Cl2 (6×30 mL)
2. dry with materialThe organic solution was dried over MgSO4
3. filtrationfiltered
4. customevaporated
5. customto give a residue
6. customThe material was purified by chromatography on SiO2 with 3% NH3-MeOH