HRID65544

反应详情

EQUATION

反应方程式

HRID 65544 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

15.2 ml of benzaldehyde and 7.51 g of 4-carboxybenzaldehyde are dissolved in 746 ml of boiling propionic acid, treated dropwise with 13.9 ml of pyrrole, the mixture obtained is subsequently heated under reflux for about 30 minutes and then left to cool to room temperature. The porphine derivative is precipitated by the addition of 0.5 l of water. The filtered-off crude product is pre-purified by two-fold column chromatography on 1.2 kg of silica gel, in each case the elution being carried out with the following solvents in sequence: chloroform/cyclohexane (1:1), chloroform/ethyl acetate (3:2) and (1:1), ethyl acetate and ethyl acetate which contains 2% methanol. For the further purification, the product is suspended in a small amount of methanol and filtered off. This procedure is repeated until the filtrate is only faintly coloured. The thus-obtained product is then chromatographed on a silica gel column using chloroform, chloroform/ethyl acetate (1:1) and ethyl acetate as the elution agent. There are obtained 1.7 g of 4-(10,15,20-triphenyl-21H,23H-porphin- 5-yl)benzoic acid as violet crystals.

WORKUP

后处理

  1. customthe mixture obtained
  2. temperatureis subsequently heated
  3. temperatureunder reflux for about 30 minutes
  4. waitleft
  5. customThe porphine derivative is precipitated by the addition of 0.5 l of water
  6. customThe filtered-off crude product is pre-purified by two-fold column chromatography on 1.2 kg of silica gel, in each case
  7. washthe elution
  8. customFor the further purification
  9. filtrationfiltered off
  10. customThe thus-obtained product is then chromatographed on a silica gel column