HRID1873065
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
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
- customTo a 250 mL flask equipped with a magnetic stirrer
- temperatureThe mixture was refluxed for one hour
- distillationThe excess POCl3 was distilled under reduced pressure
- additionThe residue was poured into water
- filtrationThe crystalline material was filtered
- customdried at