反应详情

A 50 ml 3-necked round bottom flask, equipped with a thermometer, a reflux condenser topped with a N2 inlet, a stopper and a magnetic stirrer, was charged with 3.50 g (0.0137 mole) of 3-chloro-5-iodo-2-pyridinol, from STEP 1 above, 3.00 g (0.0144 mole) of phosphorus pentachloride and 5-10 ml of phosphorus oxychloride. The reaction mixture was heated to reflux and the solid dissolved resulting in a golden brown solution. The reaction mixture was stirred under N2 at reflux for 4 hours and then cooled to room temperature. The reaction mixture was poured into crushed ice and allowed to stand for about 1 hour. A tan precipitate, which was shown to be product and unreacted starting material, formed and was isolated by filtration and washed with pentane. The aqueous layer was also washed with pentane. The combined organic layers were washed with deionized water and saturated NaCl, dried over anhydrous MgSO4, filtered and evaporated to dryness to give 0.4 g of a dark oil that crystallized upon standing.

1. customA 50 ml 3-necked round bottom flask, equipped with a thermometer, a reflux condenser
2. customtopped with a N2 inlet
3. temperatureThe reaction mixture was heated
4. temperatureto reflux
5. dissolutionthe solid dissolved
6. customresulting in a golden brown solution
7. temperatureat reflux for 4 hours
8. additionThe reaction mixture was poured
9. custominto crushed ice
10. customformed
11. customwas isolated by filtration
12. washwashed with pentane
13. washThe aqueous layer was also washed with pentane
14. washThe combined organic layers were washed with deionized water and saturated NaCl
15. dry with materialdried over anhydrous MgSO4
16. filtrationfiltered
17. customevaporated to dryness