Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Ammonia | HCID 222 | — |
| Reactant | Sodium Chloride | HCID 5234 | — |
| Reactant | HCID 10320817 | HCID 10320817 | — |
| Solvent | Ethylene Glycol | HCID 174 | — |
| Product | HCID 10318148 | HCID 10318148 | — |
Reaction Steps
Analogously to Example 1, 393 mg (0.9 mmol) of 4,5-bis(4-methoxyanilino)phthalic acid dimethyl ester in 25 ml of ethyleneglycol are heated at 120°, ammonia gas being passed through the mixture, with stirring, for 18 hours. The reaction mixture is cooled, saturated with sodium chloride and extracted with ethyl acetate. The ethylacetate phases are washed in succession three times with water and once with saturated sodium chloride solution, dried with sodium sulfate and concentrated by evaporation. The evaporation residue is chromatographed onsilica gel with ethyl acetate/hexane 1:1 and the product fractions are combined and concentrated by evaporation, yielding the title compound in the form of yellow crystals, m.p. 191°-193° C., FAB-MS: 390 [M+ +H].
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US05491144 |
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| Source dataset | uspto-grants-1996_02 |
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| ORD ID | ord-93e26cbb1f4a4ff8964eac227e45ab75 |
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| Source note | uspto-grants-1996_02 |
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