反应详情

温度

2.5 °C

Methanesulphonyl chloride (76 kg) was added to the mixture of cyclopropyl methanol (50 kg) and triethylamine (192 L) in DMF (400 L) maintained at 0-5° C., the reaction mixture was maintained at 0-5° C. for 3.0 hrs. Lithium bromide (60 Kg) was added to reaction mixture at 0-15° C. and maintained for 10-15 minutes. Noroxymorphone (40 Kg) was added to above reaction mixture at 0-5° C. and temperature raised to 65-70° C. over 1.0 hr period and maintained for 14-15 hrs. After completion of reaction it was quenched in ice-water below 20° C. and the product was extracted with ethylacetate. The ethylacetate layer was concentrated and the product was isolated with MDC and cyclohexane mixture at 10-15° C. Yield=35.3 Kg.

1. temperaturethe reaction mixture was maintained at 0-5° C. for 3.0 hrs
2. temperaturemaintained for 10-15 minutes
3. temperaturetemperature raised to 65-70° C. over 1.0 hr period
4. temperaturemaintained for 14-15 hrs
5. customAfter completion of reaction it
6. customwas quenched in ice-water below 20° C.
7. extractionthe product was extracted with ethylacetate
8. concentrationThe ethylacetate layer was concentrated
9. customthe product was isolated with MDC and cyclohexane mixture at 10-15° C