HRID1765347

反应详情

EQUATION

反应方程式

HRID 1765347 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

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 tetrahydrofuran (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 ethyl acetate (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

  1. temperatureto reflux for 24 hours
  2. customconsumption of starting material
  3. concentrationthe reaction mixture was concentrated under vacuum
  4. dissolutionThe residue was re-dissolved in ethyl acetate (50 ml)
  5. washwashed with water (2×30 ml)
  6. dry with materialthe organic layer was dried (MgSO4)
  7. filtrationfiltered
  8. concentrationconcentrated under vacuum