Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Pyridine | HCID 1049 | — |
| Reactant | Caprolactam | HCID 7768 | — |
| Reactant | 3,5-Bis(4-nitrophenoxy)benzoyl chloride | HCID 18988729 | — |
| Solvent | Benzene | HCID 241 | — |
| Product | HCID 18988726 | HCID 18988726 | 65% |
Reaction Steps
A solution of ε-caprolactam (14.82 g, 0.131 mol) in 400 ml of benzene is added to the above reactor containing 0.131 mol of 3,5-bis(4-nitrophenoxy)benzoyl chloride. The mixture is heated to 80°-90° C., and after all the reactants are dissolved, 150 ml of pyridine is added. The solution is stirred at 90° C. for 3 hours and the pyridine/acid chloride salt removed by filtration, the filtrate being kept in a freezer. White crystals formed from the filtrate are collected by filtration and dried. In order to remove traces of the 3,5-bis(4-nitrophenoxy)benzoic acid, the product is further purified by chromatography using silica gel as filler and ethyl acetate as eluate to yield 65 percent of white crystals: mp 157°-158° C.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US05491200 |
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| Source dataset | uspto-grants-1996_02 |
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| ORD ID | ord-55670efed41c489c908fb06f8d21546d |
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| Source note | uspto-grants-1996_02 |
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