Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Azane;hydrate | HCID 12896473 | — |
| Reactant | (2Z)-4-[(4-Aminophenyl)amino]-4-oxo-2-butenoic acid | HCID 18873877 | — |
| Solvent | Water | HCID 962 | — |
| Product | HCID 86708824 | HCID 86708824 | 79% |
Reaction Steps
Under a nitrogen atmosphere, into a reaction vessel were charged 12.1 g (58.7 mmol) of (2Z)-4-[(4-aminophenyl)amino]-4-oxo-2-butenoic acid and 50 ml of water. A solution prepared by dissolving 12 ml of 25% ammonia water in 12 ml of water was dropped into this under cooling with ice over a period of 15 minutes. After completion of dropping, the solvent was distilled off under reduced pressure to obtain a residue to which 100 ml of tetrahydrofuran was added, and the mixture was stirred at 50° C. for 1 hour. Thereafter, the mixture was cooled down to room temperature, the deposited solid was isolated by filtration, and washed three times with 20 ml of tetrahydrofuran. The resultant solid was dried to obtain 11.1 g of ammonium (2Z)-4-[(4-aminophenyl)amino]-4-oxo-2-butenoate mono-hydrate as a gray-green powder. Yield: 79%.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US09365497B2 |
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| Source dataset | uspto-grants-2016_06 |
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| ORD ID | ord-f9f79648793d4d2bab2f1a0c1ccb7b89 |
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| Source note | uspto-grants-2016_06 |
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