HRID1873065

反应详情

EQUATION

反应方程式

HRID 1873065 的结构方程式

PROCEDURE

实验过程

To a 250 mL flask equipped with a magnetic stirrer was added 10 g of 2-hydroxy-4-methyl-3-pyridinylcarbonitrile (8) and 60 mL of phosphorous oxychloride. The mixture was refluxed for one hour. The excess POCl3 was distilled under reduced pressure. The residue was poured into water. The crystalline material was filtered and dried at to give 10.2 g (89.2%) of (9). m.p.: 109-110° C., NMR (DMSO); ppm: 2.56 (s,3H); 7.6 (bs,1H); 8.56 (m,1H).

WORKUP

后处理

  1. customTo a 250 mL flask equipped with a magnetic stirrer
  2. temperatureThe mixture was refluxed for one hour
  3. distillationThe excess POCl3 was distilled under reduced pressure
  4. additionThe residue was poured into water
  5. filtrationThe crystalline material was filtered
  6. customdried at