HCID 136331680, compound → HCID 136331682, compound

Participants

Reaction Steps

The following is a refined version of the standard procedure (Gross et al. (2001) Inorg. Chem., 40: 4762) designed to minimize exposure of the reaction mixture to moisture and air. A Schlenk flask was equipped with a reflux condenser and all essential inlets and outlets at the beginning of the procedure. A solution of CeI[N(SiMe3)2]2 was prepared in situ by reaction of CeI3 (75.0 mg, 0.144 mmol) and LiN(SiMe3)2 (288 μL, 0.288 mmol, 1.0 M in THF) in bis(2-methoxyethyl) ether (1.5 mL). This flask was not opened. A deaerated solution of porphyrin 12 (25.0 mg, 28.9 μmol) in bis(2-methoxyethyl) ether (1 mL) was added by syringe. The mixture was refluxed for 1 h, affording the metalated porphyrin as determined by UV/Vis. Then the double-decker complex (TTP)Eu(t-Bu4Pc) (45.2 mg, 28.9 μmol) was added. The mixture was refluxed for 6 h. After cooling to room temperature, chromatography [silica, toluene/hexanes (1:1), then CH2Cl2] gave three bands (green). The first and second band were combined and concentrated, affording a solid, which was further purified by SEC (THF), affording a brownish-green solid (40 mg, 54%): A 1H NMR spectrum was recorded, but the complexity due to the mixture of regioisomers prevented a complete interpretation. LD-MS obsd 2557.5 [M+], 2542.9, 2459.8, 2431.7 [M+-I]; FAB-MS obsd (LR) 2559.86, calcd exact mass 2559.72 (C147H123CeEuIN16Si); λabs363, 421, 425, 492, 560, 609 nm.

Provenance & Evidence