HRID346922

反应详情

EQUATION

反应方程式

HRID 346922 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

6-Methoxy-2H-isoquinolin-1-one (5.0 g, 28.4 mmol) in POCl3 (10 mL) was heated to gentle reflux for 3 h the evaporated in vacuo (Nicolas Briet et al, Tetrahedron, 2002, 5761–5766). The residue was poured into iced water (20 mL) and neutralized to pH 10 with 10 M NaOH. Extracted with CHCl3. The organic layer was washed with brine, dried over MgSO4, filtered, evaporated. The residue was purified by flash chromatography (1:1 hexane-EtOAc) to afford 4.41 g (80%) of the desired product as a white solid.

WORKUP

后处理

  1. temperatureto gentle reflux for 3 h the
  2. customevaporated in vacuo (Nicolas Briet et al, Tetrahedron, 2002, 5761–5766)
  3. additionThe residue was poured into iced water (20 mL)
  4. extractionExtracted with CHCl3
  5. washThe organic layer was washed with brine
  6. dry with materialdried over MgSO4
  7. filtrationfiltered
  8. customevaporated
  9. customThe residue was purified by flash chromatography (1:1 hexane-EtOAc)