HRID1817307

反应详情

EQUATION

反应方程式

HRID 1817307 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a solution of 5-amino-2-(4-fluorobenzyl)-8-methoxy-3,4-dihydro-2,6-naphthyridin-1(2H)-one (0.889 g, 2.95 mmol) in pyridine (5 mL) was added dropwise methanesulfonyl chloride (0.575 g, 5.016 mmol). After stirring for an hour at room temperature, the product mixture was quenched with pH 7 buffer, then concentrated under vacuum. The residue was dissolved in CHCl3 and pH 7 buffer, the pH of the aqueous layer was adjusted to pH 5 with 1N NaOH and the layers separated. Several more extractions with CHCl3 were performed. The organic extracts were dried with Na2SO4, filtered, and concentrated under vacuum, then dissolved in toluene and CHCl3 and evaporated to provide the title compound.

WORKUP

后处理

  1. customthe product mixture was quenched with pH 7 buffer
  2. concentrationconcentrated under vacuum
  3. dissolutionThe residue was dissolved in CHCl3
  4. customthe layers separated
  5. extractionSeveral more extractions with CHCl3
  6. dry with materialThe organic extracts were dried with Na2SO4
  7. filtrationfiltered
  8. concentrationconcentrated under vacuum
  9. dissolutiondissolved in toluene
  10. customCHCl3 and evaporated