反应详情

温度

50 °C

To 3 (44.64 g, 117 mmol) was added reagent grade ethanol (1200 mL), glacial acetic acid (20.65 mL) and hydrazine (26 mL). The reaction mixture was stirred at 50° C. for 5 hrs. Solvent was removed and to the crude product was added methylene chloride (1,500 ml) and 1 N sodium hydroxide (67 ml) with stirring at room temperature for 15 minutes. The two resulting layers were separated and the organic layer was washed with brine (2×300 mL), dried over anhydrous sodium sulfate, filtered and solvent removed in vacuo to obtain 1-trityl-2-aminoimidazole, 4 (37.2 g, 97%). M.p. 196-199° C.

1. customSolvent was removed and to the crude product
2. additionwas added methylene chloride (1,500 ml) and 1 N sodium hydroxide (67 ml)
3. stirringwith stirring at room temperature for 15 minutes
4. customThe two resulting layers were separated
5. washthe organic layer was washed with brine (2×300 mL)
6. dry with materialdried over anhydrous sodium sulfate
7. filtrationfiltered
8. customsolvent removed in vacuo