反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
PROCEDURE
实验过程
In this example, 125 g of powdered D-glucose is added to a stirred solution of 120 ml of concentrated 96 wt.% sulfuric acid in 3 liters of acetone and the mixture is stirred vigorously at room temperature overnight. The reaction mixture is cooled to 10° C. and gaseous ammonia is bubbled keeping the temperature below 25° C. Solids are filtered off and the filtrate is concentrated under reduced pressure. The residue is treated with 1 liter of water and extracted three times with 300 ml of methylene chloride. The methylene chloride extracts are combined, washed with water, dried with annydrous magnesium sulfate, and concentrated to give a white crystalline residue of crude 1,2:5,6-di-O-isopropylidene-alpha-D-glucofuranose.
WORKUP
后处理
- temperatureThe reaction mixture is cooled to 10° C.
- customgaseous ammonia is bubbled
- customthe temperature below 25° C
- filtrationSolids are filtered off
- concentrationthe filtrate is concentrated under reduced pressure
- additionThe residue is treated with 1 liter of water
- extractionextracted three times with 300 ml of methylene chloride
- washwashed with water
- dry with materialdried with annydrous magnesium sulfate
- concentrationconcentrated