HRID494146

反应详情

EQUATION

反应方程式

HRID 494146 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A solution of 10-(benzyloxy)-4-bromo-2-(4-fluorobenzyl)-8-methyl-7,8-dihydropyrazino[1′,2′:1,5]pyrrolo[2,3-d]pyridazine-1,9(2H,6H)-dione (133 mg, 0.26 mmol) and sodium thiomethoxide (73 mg, 1.04 mmol) in anhydrous DMF (2.6 mL) was stirred at room temperature for 2 hours. The product mixture was concentrated under vacuum and the residue partitioned between chloroform and dilute hydrochloric acid. The organic phase was washed with brine, dried over anhydrous magnesium sulfate, filtered, and concentrated under vacuum. The residue was subjected to column chromatography on silica gel eluting with ethyl acetate. Collection and concentration of appropriate fractions afforded the title compound.

WORKUP

后处理

  1. concentrationThe product mixture was concentrated under vacuum
  2. customthe residue partitioned between chloroform and dilute hydrochloric acid
  3. washThe organic phase was washed with brine
  4. dry with materialdried over anhydrous magnesium sulfate
  5. filtrationfiltered
  6. concentrationconcentrated under vacuum
  7. customCollection and concentration of appropriate fractions