HRID2369642

反应详情

EQUATION

反应方程式

HRID 2369642 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

Trifluoromethanesulfonic anhydride (5.32 g, 18.9 mmol) was added dropwise to a solution of 6-hydroxy-5-methoxycarbonyl-3-phenyl-3-(4-pyrrolidinophenyl)-2H-naphtho-[1,2-b]pyran (4.8 g, 10 mmol) and pyridine (1.7 g, 21.6 mmol) in DCM (100 mL) at 0° C. under N2 with stirring. After 1 h the resulting solution was washed with HCl (100 mL, 2 M), water (100 mL), dried (MgSO4) and the solvent removed under reduced pressure. The residue was filtered through a short plug of silica using DCM as eluent. The solvent was removed under reduced pressure to give the title compound (3.57 g, 58%) as a blue powder.

WORKUP

后处理

  1. washAfter 1 h the resulting solution was washed with HCl (100 mL, 2 M), water (100 mL)
  2. dry with materialdried (MgSO4)
  3. customthe solvent removed under reduced pressure
  4. filtrationThe residue was filtered through a short plug of silica
  5. customThe solvent was removed under reduced pressure