反应详情

温度

12.5 °C

To the 20 g of thick oil of Gemcitabine base obtained as in example 3 was added 1,4-Dioxane (120 ml) and the mixture was heated to 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 was filtered off and washed with 1,4-Dioxane and dried under vacuum at 55-60° C. to get 8 g material with Specific Optical Rotation i.e.[α]D=+40° and HPLC purity of 85% β-anomer and 8% α-anomer.

1. temperaturethe mixture was heated to 60°-68° C.
2. temperaturethe contents were heated at same temperature for one hour
3. customReaction mass
4. temperaturemaintained for 30 minutes
5. customThe solid thus obtained
6. filtrationwas filtered off
7. washwashed with 1,4-Dioxane
8. customdried under vacuum at 55-60° C.