HRID1720847

反应详情

EQUATION

反应方程式

HRID 1720847 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

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.

WORKUP

后处理

  1. customThe solvent is removed by vacuum
  2. extractionthe residue is thoroughly extracted with water (3×150 ml)
  3. customall solids are removed by filtration
  4. concentrationThe resulting aqueous solution is concentrated under vacuum to 75 ml
  5. customto form a precipitate
  6. waitto settle overnight
  7. filtrationsuspension is filtered
  8. dry with materialthe solid material is dried over CaSO4