反应详情

温度

64 °C

To the 20 g of thick oil of Gemcitabine base as obtained in example 3 was added Monoglyme (120 ml) and the mixture was heated at 60-68°C. and stirred for 15 minutes. Conc. HCl (10 ml) was then added to the mixture and the contents were heated at same temperature for one hour. Reaction mass was then cooled to 10-15° C. and maintained for 30 minutes. The solid thus obtained is filtered off and washed with Monoglyme and dried under vacuum at 55-60° C. to get 8 g material having HPLC purity with 85% β-anomer & 9% α-anomer, Specific Optical Rotation i.e.[α]D=+40°

1. temperaturethe contents were heated at same temperature for one hour
2. customReaction mass
3. temperaturewas then cooled to 10-15° C.
4. temperaturemaintained for 30 minutes
5. customThe solid thus obtained
6. filtrationis filtered off
7. washwashed with Monoglyme
8. customdried under vacuum at 55-60° C.