反应方程式
[OH:1][CH2:2][CH:3]([CH2:5][OH:6])[OH:4].C1C([N+]([O-])=O)=CC=C([O:16][P:17](O)([OH:19])=[O:18])C=1.C(O)C>C(OC)(C)(C)C>[P:17]([O:1][CH2:2][CH:3]([CH2:5][OH:6])[OH:4])([OH:19])([OH:18])=[O:16]参与物
试剂、催化剂与溶剂 1
实验过程
Glycerol (10 mmol; 0.92 g) is adsorbed to an approximately equal amount of silica gel (1.0 g) and then suspended in 20 ml of t-BuOMe. To this mixture is added p-nitrophenylphosphate (10 mmol) followed by acid phosphatase from potato (1000 U; 200 mg). The mixture is stirred at room temperature for 24 hours. The solvent is removed by vacuum, the residue is thoroughly extracted with water (3×150 ml), and all solids are removed by filtration. The resulting aqueous solution is concentrated under vacuum to 75 ml and treated with a solution 21 mmol of BaCl2.2H2O to form a precipitate. To the suspension is added 500 ml of 95% ethanol and the precipitate is allowed to settle overnight. The. suspension is filtered and the solid material is dried over CaSO4. Glycerol-1-phosphate (8.5 mmol) is obtained containing 94% of the title compound as the barium salt.
后处理
- customThe solvent is removed by vacuum
- extractionthe residue is thoroughly extracted with water (3×150 ml)
- customall solids are removed by filtration
- concentrationThe resulting aqueous solution is concentrated under vacuum to 75 ml
- customto form a precipitate
- waitto settle overnight
- filtrationsuspension is filtered
- dry with materialthe solid material is dried over CaSO4
来源与证据
- ORD记录
- ord-5d1a762f90b04aa583ec61654ba283db
- 来源数据集
- uspto-grants-1996_04
- 专利号
- US05508182
关联笔记
加载中…