HRID639889

反应详情

EQUATION

反应方程式

HRID 639889 的结构方程式

PROCEDURE

实验过程

A mixture of 6-methoxy-1-oxo-4-phenyl-1,2-dihydroisoquinoline-3-carbonitrile (200 mg) and POCl3 (10 mL) was heated to 90 C for 18 h. The reaction was concentrated, and the residue was dissolve in EtOAc, cooled to 0 C, and quenched by careful addition of saturated aqueous sodium bicarbonate. The mixture was partitioned between saturated aqueous sodium bicarbonate and EtOAc. The aqueous solution was washed twice with EtOAc. The combined organic solutions were dried (Na2SO4) and concentrated. Flash chromatography (25 g silica, 3-30% EA/hex) gave a white solid.

WORKUP

后处理

  1. temperaturewas heated to 90 C for 18 h
  2. concentrationThe reaction was concentrated
  3. dissolutionthe residue was dissolve in EtOAc
  4. temperaturecooled to 0 C
  5. customquenched by careful addition of saturated aqueous sodium bicarbonate
  6. customThe mixture was partitioned between saturated aqueous sodium bicarbonate and EtOAc
  7. washThe aqueous solution was washed twice with EtOAc
  8. dry with materialThe combined organic solutions were dried (Na2SO4)
  9. concentrationconcentrated
  10. customFlash chromatography (25 g silica, 3-30% EA/hex) gave a white solid