反应详情

In a three-necked flask protected from light, butyltriphenyltin (21.05 g; 51.8 mmol) was dissolved in 50 mL of dry methanol. A solution of iodine (12.06 g; 47.5 mmol) in methanol was then added slowly. After stirring at room temperature during 16 hours, methanol was eliminated under vacuum. The residue was dissolved in petroleum ether and washed with a saturated aqueous solution of sodium thiosulphate. Organic layers were washed with a saturated NaCl solution and dried over MgSO4. Solvent was evaporated and the crude product was distilled using a Kugelrohr apparatus at 60° C. A colourless oil was obtained (22.2 g, 48.6 mmol).

1. washwashed with a saturated aqueous solution of sodium thiosulphate
2. washOrganic layers were washed with a saturated NaCl solution
3. dry with materialdried over MgSO4
4. customSolvent was evaporated
5. distillationthe crude product was distilled
6. customat 60° C
7. customA colourless oil was obtained (22.2 g, 48.6 mmol)