反应详情

A 100-mL eggplant shaped flask was charged with 1.0 g of sodium 2,4,6-tricyclohexylbenzoate (prepared in Synthesis Example 1-6), 0.9 g of 10-phenyl-10-phenoxathiinium methylsulfate (prepared in Synthesis Example 1-8), 10 g of methyl isopropyl ketone, 10 g of 1-pentanol, and 5 g of water, which were stirred at room temperature for 1 hour. The organic layer was separated from the reaction mixture and washed with water. After washing, the organic layer was concentrated by distilling off the solvent. The liquid concentrate was crystallized from 30 g of diisopropyl ether. The crystal precipitate was filtered and dried, obtaining the target compound, 10-phenyl-10-phenoxathiinium 2,4,6-tricyclohexylbenzoate as white crystal. Amount 1.4 g, yield 88%.

1. customThe organic layer was separated from the reaction mixture
2. washwashed with water
3. washAfter washing
4. concentrationthe organic layer was concentrated
5. distillationby distilling off the solvent
6. concentrationThe liquid concentrate
7. customwas crystallized from 30 g of diisopropyl ether
8. filtrationThe crystal precipitate was filtered
9. customdried