Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Ethylenediamine | HCID 3301 | — |
| Reactant | Sodium Bicarbonate | HCID 516892 | — |
| Reactant | Ethanol hydrochloride | HCID 21887872 | — |
| Reactant | HCID 21939849 | HCID 21939849 | — |
| Solvent | Ethanol | HCID 702 | — |
| Product | HCID 21940017 | HCID 21940017 | — |
Reaction Steps
10.1 N Hydrogen chloride-ethanol solution (30 ml) was added to an ethanol suspension of N-[4-[(E)-2-cyanoethenyl]phenyl][1,1′-biphenyl]-4-carboxamide (250 mg, 0.771 mmol) obtained in Reference Example under room temperature, which was stirred for 16 hours. After the solvent was distilled out under reduced pressure, ethanol was again added to the residue, and then ethylenediamine (0.155 ml, 2.31 mmol) was added at room temperature, which was stirred for 16 hours. Sodium hydrogencarbonate solution was added to the reaction mixture, and the precipitated crude product was washed with water and chloroform. This product was dissolved in methanol. 1 N Hydrochloric acid (4 ml) was added to the solution, and the solvent was distilled out under reduced pressure. Small amount of water was added to the resulting residue, to give the titled compound (124 mg) as a colorless powder.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US07115750B1 |
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| Source dataset | uspto-grants-2006_10 |
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| ORD ID | ord-f9b6fa84e83b434981c7de4b63e731e2 |
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| Source note | uspto-grants-2006_10 |
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