反应详情

温度

80 °C

5.0 g of 3-bromo-tetrahydropyran-2-ol prepared in Example 1 and 5.75 g of formamidine acetate were added to 25 ml of N,N-dimethylformamide and 9 ml of diethylamine was added dropwise thereto. The reaction mixture was stirred for about 4 hours at 80° C. and distilled in vacuo for about 1 hour at the same temperature to remove the solvent. The resulting oily residue was diluted with 25 ml of acetone and 4.97 g of oxalic acid was slowly added thereto for crystallization. The reaction mixture was stirred for about 1 hour, filtered, and washed with acetone to give 2.5 g of 3-(1H-imidazol-4-yl)propanol oxalate (yield: 42%).

1. additionwas added dropwise
2. distillationdistilled in vacuo for about 1 hour at the same temperature
3. customto remove the solvent
4. additionThe resulting oily residue was diluted with 25 ml of acetone and 4.97 g of oxalic acid
5. additionwas slowly added
6. customfor crystallization
7. stirringThe reaction mixture was stirred for about 1 hour
8. filtrationfiltered
9. washwashed with acetone