Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Water | HCID 962 | — |
| Reactant | Pyridine | HCID 1049 | — |
| Reactant | Isophthaloyl chloride | HCID 7451 | — |
| Reactant | HCID 58979972 | HCID 58979972 | — |
| Solvent | Methanol | HCID 887 | — |
| Solvent | Chloroform | HCID 6212 | — |
| Solvent | Hexane | HCID 8058 | — |
| Product | HCID 57865058 | HCID 57865058 | 84% |
Reaction Steps
After dissolving 5.0 g of 2-(2H-tetrazole-5-yl)-1,10-phenanthroline into 50 ml of dehydrated pyridine, 2.1 g of isophthaloylchloride was added. The mixture was heated to 100° C. and stirred under reflux for 5 hours. After cooling to a room temperature, the reaction solution was poured into water to collect a precipitated solid by suction filtration, and the solid was washed with water. The solid was dried under vacuum at 70° C. for 20 hours to obtain a brownish crude product. After dissolving the thus-obtained crude product into a mixed solution of chloroform:methanol=4:1, hexane was added to allow purification by crystallization, thereby obtaining 4.82 g of PhenOXDm (2) (yield: 84%). NMR analysis (see FIG. 1) was performed for identification of the product. The results of the NMR analysis are as follows. 9.15 ppm (2H), 8.89 ppm (1H), 8.73 ppm (2H), 8.59 ppm (2H), 8.50 ppm (2H), 8.45 ppm (2H), 8.07 ppm (4H), 7.97 ppm (1H), 7.78 ppm (2H).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US08247087B2 |
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| Source dataset | uspto-grants-2012_08 |
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| ORD ID | ord-4ba72352171a4ba1832a35c72f1ad41f |
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| Source note | uspto-grants-2012_08 |
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