反应详情

Under an argon atmosphere, to a solution of 8.04 g (18 mmol) of tetraethyl 2-naphthylthiomethane-diphosphonate obtained in Example 1 in dry methylene chloride (100 ml) was added dropwise 27.56 g (180 mmol) of trimethylsilyl bromide at room temperature and then the mixture was stirred at room temperature for 72 hours. After the solvent and the excess trimethylsilyl bromide were distilled off under reduced pressure, the resulting residue was dissolved in a mixed solvent of water:methanol=5:95, and the solution was heated to reflux for 30 minutes, and the solvent was again distilled off under reduced pressure. The resulting residue was crystallized from acetone/methylene chloride and the obtained crystals were recrystallized from the same solvent to obtain the title compound as white crystals. The yield was 86%.

1. distillationAfter the solvent and the excess trimethylsilyl bromide were distilled off under reduced pressure
2. dissolutionthe resulting residue was dissolved in a mixed solvent of water
3. temperaturemethanol=5:95, and the solution was heated
4. temperatureto reflux for 30 minutes
5. distillationthe solvent was again distilled off under reduced pressure
6. customThe resulting residue was crystallized from acetone/methylene chloride
7. customthe obtained crystals were recrystallized from the same solvent