反应详情

5,10,15,20-tetrakis-(4-Hydroxy-phenyl)-porphyrin (100 mg, 0.15 mmol) is dissolved and K2CO3 (230 mg) is suspended in DMF (30 mL). To the vigorously stirred reaction mixture a solution of 1-bromodecane (0.016 mL, 0.11 mmol) in DMF (10 mL) is added dropwise at 70° C. during 30 mins and the mixture is stirred for 1.5 h. After evaporation of solvent, the residue is dissolved in toluene:ethanol (1:1 by vol., ca. 3 mL) and purified by chromatography on a column (150 g) of silica gel (Merck 60) using toluene as eluent. After elution of the first 3 fractions, the column is eluted with toluene:ethyl acetate (2:1 by vol.) and the 5th fraction eluted is collected, the solvent removed and the residue dried under high vacuum to give the product as violet crystals.

1. additionis added dropwise at 70° C. during 30 mins
2. customAfter evaporation of solvent
3. dissolutionthe residue is dissolved in toluene:ethanol (1:1 by vol., ca. 3 mL)
4. custompurified by chromatography on a column (150 g) of silica gel (Merck 60)
5. washAfter elution of the first 3 fractions
6. washthe column is eluted with toluene:ethyl acetate (2:1 by vol.)
7. washthe 5th fraction eluted
8. customis collected
9. customthe solvent removed
10. customthe residue dried under high vacuum