反应详情

温度

0 °C

0.4 grams of 1-(4-bromopyrid-3-yl)-1-(4-chloropyrid-3-yl)methanol were dissolved in 50 ml of tetrahydrofuran (THF) and cooled to 0° C. One gram of trimethylacetyl chloride was added followed by the portionwise addition of 0.5 grams of sodium hydride (60%) over a period of 15 minutes. The reaction mixture was then allowed to warm to room temperature and then stirred overnight. 50 ml of a saturated ammonium chloride solution were added and then this mixture was extracted twice with ethyl ether. The combined ether extracts were washed with a 5% aqueous solution of potassium carbonate, dried over magnesium sulfate, filtered, and concentrated in vacuo to afford 0.5 g of 1-(4-bromopyrid-3-yl)-1-(4-chloropyrid-3-yl)-1-trimethylacetoxymethane as a waxy solid.

1. temperatureto warm to room temperature
2. extractionthis mixture was extracted twice with ethyl ether
3. washThe combined ether extracts were washed with a 5% aqueous solution of potassium carbonate
4. dry with materialdried over magnesium sulfate
5. filtrationfiltered
6. concentrationconcentrated in vacuo