反应详情

温度

-70 °C

To a solution of 4.0 ml (0.088 mole) of chlorine in 200 ml of methylene chloride cooled to -70° C. is added dropwise a solution of 7.65 g (0.088 mole) of methylthioacetonitrile in 1 liter of methylene chloride while maintaining the temperature below -65° C. After several minutes a solution containing 0.2 mole of 2-amino-5-methoxybenzophenone in 100 ml of methylene chloride is added dropwise over a 30 min period. The mixture is stirred at -70° C. for about 1.5 hr and 18 g (0.18 mole) of triethylamine is added. The mixture is stirred for about an hour at -70° C. and then allowed to warm to ambient temperature. The mixture is washed with water, dried over sodium sulfate and concentrated under reduced pressure. The residue is recrystallized from a suitable solvent, e.g., 2-propanol, to give the title product.

1. temperaturewhile maintaining the temperature below -65° C
2. additionis added dropwise over a 30 min period
3. stirringThe mixture is stirred for about an hour at -70° C.
4. temperatureto warm to ambient temperature
5. washThe mixture is washed with water
6. dry with materialdried over sodium sulfate
7. concentrationconcentrated under reduced pressure
8. customThe residue is recrystallized from a suitable solvent, e.g., 2-propanol