反应详情

Dihydrophytol (0.60 g) and bromoethyl phosphorodichloridate (0.83 g) were dissolved in dry benzene (10 ml). To the solution was added dropwise dry pyridine (0.2 ml) under stirring. The mixture was stirred at room temperature for three hours, then cooled with ice, to which was added 2 ml of water. The mixture was again stirred vigorously at room temperature for two hours. The solvent was evaporated off, and the residue was dissolved in ether. The ether solution was washed with water, and then concentrated to dryness. The residue was dissolved in toluene (10 ml) containing trimethylamine (2 g), and the solution was left standing for five days. The reaction solution was concentrated under reduced pressure. The residue was subjected to a silica-gel chromatography (eluent, methanol) to yield 0.404 g (43%) of the object compound as colorless solid matter.

1. stirringThe mixture was stirred at room temperature for three hours
2. temperaturecooled with ice, to which
3. stirringThe mixture was again stirred vigorously at room temperature for two hours
4. customThe solvent was evaporated off
5. dissolutionthe residue was dissolved in ether
6. washThe ether solution was washed with water
7. concentrationconcentrated to dryness
8. dissolutionThe residue was dissolved in toluene (10 ml)
9. additioncontaining trimethylamine (2 g)
10. waitthe solution was left
11. concentrationThe reaction solution was concentrated under reduced pressure