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温度

0 °C

In sequence, 4 mL 65% technical nitric acid and then within three hours 50 mL 98% technical sulfuric acid are added to 6.572 g (40 mmol) 1,3-dimethyladamantane at 0° C. It is stirred over night at 0° C. and the mixture is poured at 0° C. onto 100 mL formamide in a round bottom flask which is provided with a drying tube. This mixture is stirred for 30 min at 0° C. and for 90 min at room temperature and 200 mL dichloromethane and 200 mL water are added. After phase separation, the organic phase is washed with water and 2% NaHCO3-solution, is dried, over Na2SO4 and is freed from solvents at the rotary evaporator. The remaining oil is chromatographically purified (SiO2, CHCl3/acetone (20:1), Rf=0.39). 7.41 g (89.3%) of the formamide are obtained as a nearly colourless solid.

1. customis provided with a drying tube
2. stirringThis mixture is stirred for 30 min at 0° C. and for 90 min at room temperature
3. customAfter phase separation
4. washthe organic phase is washed with water and 2% NaHCO3-solution
5. dry with materialis dried, over Na2SO4
6. customis freed from solvents at the rotary evaporator
7. customThe remaining oil is chromatographically purified (SiO2, CHCl3/acetone (20:1), Rf=0.39)