反应详情

The solution of POCl3 (10 mL) and 7-methyl-isoquinolin-1-ol (3.55 g, 22.3 mmol) was refluxed under nitrogen for 5 h. The residue, after removal of POCl3 by distillation, was quenched with iced water and extracted with methylene chloride (3×). Purification by flash silica gel column using 10-25% EtOAc in hexane as elute gave 3.40 g (85% yield) of desired product. 1H-NMR (300 MHz, CDCl3) δ 8.21 (d, 1H), 8.11 (s, 1H), 7.75 (d, 1H 7.60 (d, 1H), 7.55 (d, 1H), 2.60 (s, 3H).

1. customThe residue, after removal of POCl3
2. distillationby distillation
3. customwas quenched with iced water
4. extractionextracted with methylene chloride (3×)
5. customPurification by flash silica gel column
6. washas elute