HRID2244853

反应详情

EQUATION

反应方程式

HRID 2244853 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

2.8 g (9.58 mmol) of 4,5-difluoro-2-methyl-7-pentyl-7H-furo[3,2-f]chromene are hydrogenated for a few minutes in toluene using elemental hydrogen in the presence of Pd/C (5% Pd). The reaction soln. is concentrated to dryness, and the residue is purified by column chromatography (SiO2, n-heptane:1-chlorobutane=2:1). The further purification is carried out by recrystallisation from ethanol, giving 4,5-difluoro-2-methyl-7-pentyl-8,9-dihydro-7H-furo[3,2-f]chromene as a colourless solid having an m.p. of 61° C. (Δ∈=−6.7).

WORKUP

后处理

  1. concentrationis concentrated to dryness
  2. customthe residue is purified by column chromatography (SiO2, n-heptane:1-chlorobutane=2:1)
  3. customThe further purification
  4. customis carried out by recrystallisation from ethanol