Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Dichloromethane | HCID 6344 | — |
| Reactant | N-Methylethylenediamine | HCID 8014 | — |
| Reactant | Ethyl 4-cyanobenzoate | HCID 81589 | — |
| Solvent | Hydrochloric Acid | HCID 313 | — |
| Solvent | Ethanol | HCID 702 | — |
| Solvent | 1,4-Dioxane | HCID 31275 | — |
| Product | HCID 69921167 | HCID 69921167 | — |
Reaction Steps
1.8 g (10.3 mmol) of ethyl 4-cyanobenzoate was dissolved in a mixture of 20 ml of 4 N solution of hydrogen chloride in dioxane and 5 ml of ethanol, and the obtained solution was stirred at room temperature for 3 days. The solvent was evaporated, and the residue was washed with ethyl acetate. The obtained crude product was dissolved in 20 ml of ethanol. 1.52 g (20.6 mmol) of N-methylethylenediamine was added to the obtained solution, and they were heated under reflux for 6 hours. The solvent was evaporated, and the obtained crude product was treated with dichloromethane as the extraction solvent in an ordinary manner. The obtained crude product was dissolved in 10 ml of concentrated hydrochloric acid, and the obtained solution was stirred at 50° C. overnight. The solvent was evaporated to obtain the crude title compound.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US06410538B2 |
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| Source dataset | uspto-grants-2002_06 |
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| ORD ID | ord-5e0558a20c014f36b86eac0dfd3fcd39 |
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| Source note | uspto-grants-2002_06 |
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