HRID2060858

反应详情

EQUATION

反应方程式

HRID 2060858 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
80 °C

PROCEDURE

实验过程

To 6-(1-methylisoquinolin-4-yloxy)nicotinamide (Preparation 19) (135 mg, 0.48 mmol) in dioxane (6 mL) under argon was added selenium dioxide (54 mg, 0.48 mmol). The mixture was heated to 80° C. for 3 h after which time selenium dioxide (54 mg, 0.48 mmol) was added. After a further 0.5 h at 80° C. the mixture was cooled, filtered through Celite and washed with EtOAc (50 mL). The organic phase was washed with NaHCO3 (30 mL), water (30 mL), brine (30 mL) and dried (MgSO4). Solvent was removed in vacuo to give the title compound: RT=2.93 min; m/z (ES+)=294.1 [M+H]+.

WORKUP

后处理

  1. additionwas added
  2. filtrationfiltered through Celite
  3. washwashed with EtOAc (50 mL)
  4. washThe organic phase was washed with NaHCO3 (30 mL), water (30 mL), brine (30 mL)
  5. dry with materialdried (MgSO4)
  6. customSolvent was removed in vacuo