반응 #42451

반응 방정식

4-cyanopyridine-N-oxide

phosphorus oxychloride

→

title compound

2-Chloroisonicotinonitrile

반응 조건

후처리

1. 1
   온도The mixture was cooled to room temperature
2. 2
   기타the excess phosphorus oxychloride removed under reduced pressure
3. 3
   workup.DISSOLUTIONThe residue was dissolved in water
4. 4
   추출The product was extracted into methylene chloride
5. 5
   건조dried over anhydrous magnesium sulfate
6. 6
   농축concentrated under reduced pressure

실험 절차

4-cyanopyridine-N-oxide (10.0 g) was added to phosphorus oxychloride (85 mL) and heated to 110° C. for 2.5 h. The mixture was cooled to room temperature and the excess phosphorus oxychloride removed under reduced pressure. The residue was dissolved in water and made basic with concentrated ammonia. The product was extracted into methylene chloride, dried over anhydrous magnesium sulfate and concentrated under reduced pressure. Column chromatography on silica gel (100 mL) using methylene chloride as eluent to give 7.19 g of the title compound: 1H NMR (CDCl3) δ 7.48, 7.6, 8.6.

출처