反应详情

温度

53 °C

A mixture of dry N-methylpiperidine hydrochloride (8.14 g., 0.06 mole) anhydrous ethanol free chloroform (180 ml.), 6-triphenylmethylamino-2,2-dimethyl-3-cyanopenam (13.2g., 0.03 mole), finely powdered sodium azide (3.9 g., 0.06 mole) and N-methylpiperidine (8.9 g., 0.09 mole) is heated to 53° C. (internal temperature) for 80 minutes. It is then cooled to room temperature and diluted with ethanol free chloroform (750 ml.) and water (800 ml.). It is thoroughly shaken, the chloroform phase separated and washed successively with 1.5N HCl (1 × 1000 ml.) and water (1 × 800 ml.). The chloroform solution is filtered through anhydrous sodium sulfate and then concentrated under reduced pressure to about 300 ml. White crystals separate. The concentrate is diluted with hexane (350 ml.) and filtered after 15 minutes. The crystalline product is washed with hexane and dried in air for 15 minutes followed by drying under vacuum at 56° C. for 1 hour. Yield = 7.66 g. (52.9%).

1. temperatureIt is then cooled to room temperature
2. customthe chloroform phase separated
3. washwashed successively with 1.5N HCl (1 × 1000 ml.) and water (1 × 800 ml.)
4. filtrationThe chloroform solution is filtered through anhydrous sodium sulfate
5. concentrationconcentrated under reduced pressure to about 300 ml
6. customWhite crystals separate
7. additionThe concentrate is diluted with hexane (350 ml.)
8. filtrationfiltered after 15 minutes
9. washThe crystalline product is washed with hexane
10. customdried in air for 15 minutes
11. customby drying under vacuum at 56° C. for 1 hour