HRID1783660
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
To a stirred solution of 7-hydroxy-2-Isopropyl-4-bromo-2H-phthalazin-1-one (0.4 g, 1.4 mmol) in THF (5 ml) were added successively, K2CO3 (0.59 g, 4.3 mmol) and methyl iodide (0.22 g, 1.55 mmol) and the mixture was heated to reflux for 24 hours. After this time, LC-MS indicated complete consumption of starting material, and the reaction mixture was concentrated under vacuum. The residue was re-dissolved in EtOAc (50 ml) and washed with water (2×30 ml), the organic layer was dried (MgSO4), filtered and concentrated under vacuum to give the title compound (0.32 g, 76% yield) as an orange powder.
WORKUP
后处理
- temperatureto reflux for 24 hours
- customconsumption of starting material
- concentrationthe reaction mixture was concentrated under vacuum
- dissolutionThe residue was re-dissolved in EtOAc (50 ml)
- washwashed with water (2×30 ml)
- dry with materialthe organic layer was dried (MgSO4)
- filtrationfiltered
- concentrationconcentrated under vacuum