Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Water | HCID 962 | — |
| Reactant | Propylamine | HCID 7852 | — |
| Reactant | 1,3-Propanediamine, N'-(ethylcarbonimidoyl)-N,N-dimethyl-, monohydrochloride | HCID 2723939 | — |
| Reactant | HCID 22440043 | HCID 22440043 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 53713215 | HCID 53713215 | 59.3% |
Reaction Steps
1-(3-Dimethylaminopropyl)-3-ethylcarbodiimide hydrochloride (1.45 g, 7.53 mmol) was added to a solution of Compound 93 (1.5 g, 3.76 mmol) obtained in Example 93 and propylamine (0.47 ml, 5.65 mmol) in 50 ml of methylene chloride, followed by stirring at room temperature for 4.5 hours. Water was added to the reaction solution followed by extraction with chloroform. The resulting organic layer was washed successively with water and a saturated aqueous solution of sodium chloride, and dried over magnesium sulfate, and the solvent was distilled off under reduced pressure to give a crude product. The obtained crude product was purified with silica gel column chromatography (chloroform/methanol=40/1) followed by recrystallization from diisopropyl ether to give 0.98 g (yield: 59%) of the title compound.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US05891902 |
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| Source dataset | uspto-grants-1999_04 |
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| ORD ID | ord-58b8e97d422b488984902f3c23b43fa9 |
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| Source note | uspto-grants-1999_04 |
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