HRID66076

反应详情

EQUATION

反应方程式

HRID 66076 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A solution of 52.2 g (0.223 mole) of crude 2-hydroxy-9-methoxy-2,3-dihydro-7H-furo[3,2-g][1]benzopyran-7-one in 900 ml of 98% formic acid was heated under argon at 100° for 45 min. The solvent was removed in vacuo and the dark residue crystallized. After drying on the high vac, the crude product, was taken up in the minimum amount of warm methylene chloride and filtered through an alumina column. Evaporation of fractions afforded pure methoxsalen, mp 145°-146°.

WORKUP

后处理

  1. customThe solvent was removed in vacuo
  2. customthe dark residue crystallized
  3. customAfter drying on the high vac
  4. filtrationfiltered through an alumina column
  5. customEvaporation of fractions