HuagongsheHuagongshe Chemistry Print Report · For research reference only
Triethylamine → 1,2-Dihydro-3-methyl-1-[6-[(2,2,2-trifluoro)ethanesulfonamido]hexan-1-yl)-1,4,7b-triazacyclopent[cd]inden-2-one
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Triethylamine | HCID 8471 | — |
| Reactant | 2,2,2-Trifluoroethanesulfonyl chloride | HCID 74242 | — |
| Reactant | 1-[6-(Amino)hexyl]-1,2-dihydro-3-methyl-1,4,7b-triazacyclopent[cd]inden-2-one | HCID 21190087 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | 1,2-Dihydro-3-methyl-1-[6-[(2,2,2-trifluoro)ethanesulfonamido]hexan-1-yl)-1,4,7b-triazacyclopent[cd]inden-2-one | HCID 70213150 | 77.3% |
Reaction Steps
To a solution of 676 mg (2.48 mmol) of 1-[6-(amino)hexyl]-1,2-dihydro-3-methyl-1,4,7b-triazacyclopent[cd]inden-2-one and 0.52 ml (3.73 mmol) of triethylamine in 30 ml of methylene chloride was added, while stirring under ice-cooling, 0.55 g (3.01 mmol) of 2,2,2-trifluoroethanesulfonylchloride, and the mixture was stirred for 30 minutes at the same temperature range. The reaction mixture was washed with an aqueous solution of sodium hydrogencarbonate, dried over anhydrous magnesium sulfate. The solvent was distilled off, and the residue was purified by column chromatography (eluent: ethyl acetate) to give 802 mg of the desired compound (77.2%, pale brown solid).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US05958942 |
| Source dataset | uspto-grants-1999_09 |
| ORD ID | ord-b6642e38272d48d4822d37e5136e176e |
| Source note | uspto-grants-1999_09 |