反应详情

To a vigorously-stirred suspension of 5,10,15,20-tetrakis-(4-hydroxy-phenyl)-porphyrin (400 mg, 0.59 mmol) and K2CO3 (1.0 g, 7.1 mmol) in DMF (10 mL) is added dropwise at 50° C. during 30 mins and the mixture is stirred at the same temperature for 1.5 h. After removal by filtration of K2CO3 and removal under reduced pressure of DMF, the residue obtained is dissolved in dichloromethane (200 mL), washed with water (3×150 mL) and the solution dried (Na2SO4). The solvent is evaporated under reduced pressure and the residue obtained is dissolved in toluene:ethanol (5:1 by vol., ca. 10 mL) and purified by chromatography using a column (5×5 cm) of silica gel (Merck 60). The column is eluted with toluene followed by toluene:ethyl acetate (2:1 by vol.) and the desired material recovered by evaporation of solvent from the appropriate fractions is dried under high vacuum. The product is obtained as violet crystals.

1. additionis added dropwise at 50° C. during 30 mins
2. customAfter removal
3. filtrationby filtration of K2CO3 and removal under reduced pressure of DMF
4. customthe residue obtained
5. washwashed with water (3×150 mL)
6. dry with materialthe solution dried (Na2SO4)
7. customThe solvent is evaporated under reduced pressure
8. customthe residue obtained
9. custompurified by chromatography
10. washThe column is eluted with toluene
11. customthe desired material recovered by evaporation of solvent from the appropriate fractions
12. customis dried under high vacuum
13. customThe product is obtained as violet crystals