Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | HCID 178450622 | HCID 178450622 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Product | 21H,22H-Porphine | HCID 137705241 | 6.4% |
Reaction Steps
A solution of porphyrin 40 (355 mg, 0.50 mmol) and MnCl2 (318 mg, 2.53 mmol) in anhydrous DMF (50 mL) was magnetically stirred and heated to 145° C. for 1 h then exposed to a stream of air for 2 h. The reaction mixture was cooled to room temperature overnight under a stream of air. Evaporation of DMF provided a crude solid mixture which was adsorbed onto silica gel (2 g). Purification by column chromatography (gradient elution with 0-5% MeOH/CH2Cl2) provided porphyrins 41 (170 mg) and 42 (10 mg) as solids. For porphyrin 41: mp 200-210° C.; UV-vis λmax=456.0 nm, ε=1.4×105 L/cm-mol; FAB MS m/z=763 [C40H44MnN4O8]+. For porphyrin 42: mp 200-205° C.; UV-vis λmax=459.5 nm, ε=7.2×104 L/cm-mol; FAB MS m/z=707, [C36H36MnN4O8]+.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US06479477B1 |
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| Source dataset | uspto-grants-2002_11 |
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| ORD ID | ord-86b7719936c74b4cb866912d18e6d9d2 |
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| Source note | uspto-grants-2002_11 |
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