Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Phenol | HCID 996 | — |
| Reactant | HCID 18626155 | HCID 18626155 | — |
| Reactant | 3-(Cycloundecen-1-yl)-1,2-diazacycloundec-2-ene | HCID 53630274 | — |
| Solvent | Diethyl Ether | HCID 3283 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Product | HCID 86583809 | HCID 86583809 | 33.8% |
Reaction Steps
N,N′-Carbonyldiimidazole (0.41 g, 2.5 mmol) was added to a stirred solution of 3-(phenylamino)-4-methoxybenzoic acid (0.6 g, 2.5 mmol) in dimethylformamide (15 mL) under an inert atmosphere. After 30 minutes, the solution was heated to 50° C. for 1 hour, then phenol (0.24 g, 2.6 mmol) was added followed by diazabicycloundecene (0.40 g, 2.6 mmol) and heating at 50° C. was continued for 20 more hours. The mixture was allowed to cool and was then diluted with diethyl ether (100 mL) and washed successively with 2N HCl, water, 0.5N K2CO3, and saturated brine then dried over MgSO4. The solvent was removed under reduced pressure, and the residue was chromatographed on a column of silica gel in ethyl acetate to afford the product (0.27 g); m.p. 130-131° C. after recrystallization from acetonitrile.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US06528528B2 |
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| Source dataset | uspto-grants-2003_03 |
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| ORD ID | ord-6a86ac08ba4c419bae38d43a3673e83c |
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| Source note | uspto-grants-2003_03 |
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