HRID346922
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
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
- temperatureto gentle reflux for 3 h the
- customevaporated in vacuo (Nicolas Briet et al, Tetrahedron, 2002, 5761–5766)
- additionThe residue was poured into iced water (20 mL)
- extractionExtracted with CHCl3
- washThe organic layer was washed with brine
- dry with materialdried over MgSO4
- filtrationfiltered
- customevaporated
- customThe residue was purified by flash chromatography (1:1 hexane-EtOAc)