反应详情

温度

82 °C

50ELH87 (0.3 g, 0.852 mmol, 1.0 eq) and 4-(chloromethyl)-2-methylthiazole hydrochloride (0.235 g, 1.5 eq) were added to a 7 ml vial and dissolved in acetonitrile (3 ml). Potassium carbonate (141.3 g, 1.2 eq) and a crystal of potassium iodide were added and the vial was sealed and shaken for 20 h at 82° C. The reaction mixture was extracted with distilled water (made basic by potassium carbonate, pH 10) and dichloromethane. The crude product was dried with sodium sulfate and concentrated. After purification by HPLC the product was converted into the hydrochloride salt by dissolving the free base in 1 ml dichloromethane and adding 1 eq. HCl in ether (2M). This mixture was added drop-wise to an excess of heptane where the product precipitated. The solvent was removed by evaporation leaving a white powder as the product. yield 83.8 mg (21%), UV/MS 100/90 (M+ 463), rt (B, MS) 11.82.

1. customthe vial was sealed
2. extractionThe reaction mixture was extracted with distilled water (made basic by potassium carbonate, pH 10) and dichloromethane
3. dry with materialThe crude product was dried with sodium sulfate
4. concentrationconcentrated
5. customAfter purification by HPLC the product
6. dissolutionby dissolving the free base in 1 ml dichloromethane
7. additionadding 1 eq
8. additionThis mixture was added drop-wise to an excess of heptane where the product
9. customprecipitated
10. customThe solvent was removed by evaporation
11. customleaving a white powder as the product
12. customyield 83.8 mg (21%), UV/MS 100/90 (M+ 463), rt (B, MS) 11.82