反应详情

温度

70 °C

A mixture of 120 (20 mmol), acetamidine hydrochloride (40 mmol) and K2CO3 (6.9 g, 50 mmol) in EtOH (50 ml) is heated at 70° C. overnight. The solid is filtered and the residue is dissolved in water (30 ml). Acetic acid is added to adjust the pH to 4. The mixture is then extracted with CH2Cl2 (4×50 ml) and the combined extracts are washed with brine (100 ml). The solution is dried (Na2SO4) and evaporated in vacuo to give a light yellow solid (121), which is used directly in the next step.

1. filtrationThe solid is filtered
2. dissolutionthe residue is dissolved in water (30 ml)
3. additionAcetic acid is added
4. extractionThe mixture is then extracted with CH2Cl2 (4×50 ml)
5. washthe combined extracts are washed with brine (100 ml)
6. dry with materialThe solution is dried (Na2SO4)
7. customevaporated in vacuo