HRID40189

反应详情

EQUATION

反应方程式

HRID 40189 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a mixture of 4-(2-hydroxyethyl)morpholine (0.0964 ml, 0.788 mmol),triphenylphosphine (0.238 g, 0.909 mmol), 2-fluoro-4-(3-((7-methoxyquinolin-4-yloxy)methyl)-[1,2,4]triazolo[4,3-b]pyridazin-6-yl)phenol (0.253 g, 0.606 mmol) (prepared according to General Method A) in THF (10 mL) was added DEAD (0.144 ml, 0.909 mmol). Stirred at room temperature for 1 h. Concentrated. Purified on RPHPLC. Fractions containing product were treated with 9% sodium carbonate. Removed volatiles in vacuo. Product crashed out and was isolated by filtration. MS m/z=531.2 [M+1]+. Calc'd for C28H27FN6O4: 530.5.

WORKUP

后处理

  1. concentrationConcentrated
  2. customPurified on RPHPLC
  3. additionFractions containing product
  4. additionwere treated with 9% sodium carbonate
  5. customwas isolated by filtration