Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Triethylamine | HCID 8471 | — |
| Reactant | Ethyl trifluoroacetate | HCID 9794 | — |
| Reactant | 3-Methyl-1-[5-(amino)pentyl]-1,4,7b-triazacyclopent[cd]inden-2-one | HCID 21190111 | — |
| Solvent | Acetonitrile | HCID 6342 | — |
| Product | HCID 21190163 | HCID 21190163 | — |
Reaction Steps
To a solution of 2.58 g (10.0 mmol) of 3-methyl-1-[5-(amino)pentyl]-1,4,7b-triazacyclopent[cd]inden-2-one and 1.81 ml (13.0 mmol) of triethylamine in 100 ml of acetonitrile was added, while stirring under ice-cooling, 1.43 ml (12.0 mmol) of trifluoroacetic acid ethyl ester. The mixture was stirred for one hour at the same temperature. The solvent was distilled off. To the residue was added ethyl acetate--tetrahydrofuran. The mixture was washed with an aqueous saline solution, and dried over anhydrous magnesium sulfate. The solvent was distilled off. The residue was purified by column chromatography (eluent: ethyl acetate), which was recrystallized from ethyl acetate-n-hexane to afford 2.57 g (72.6%, a pale yellow crystals) of the desired compound.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US05958942 |
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| Source dataset | uspto-grants-1999_09 |
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| ORD ID | ord-abf16d18f8cc4f338c3d0dbb111ec17c |
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| Source note | uspto-grants-1999_09 |
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