HuagongsheHuagongshe Chemistry Print Report · For research reference only
Water → HCID 21190184, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Water | HCID 962 | — |
| Reactant | Phthalimide | HCID 6809 | — |
| Reactant | Sodium hydride | HCID 24758 | — |
| Reactant | 1,2-Dihydro-3-methyl-1,4,7b-triazacyclopent[cd)inden-2-one | HCID 135810294 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Product | HCID 21190184 | HCID 21190184 | 122.1% |
Reaction Steps
To a suspension of 8.66 g (50 mmol) of 1,2-dihydro-3-methyl-1,4,7b-triazacyclopent[cd]inden-2-one in 100 ml of DMF was added, while stirring under ice-cooling, 2.20 g (55 mmol) of 60% sodium hydride (dispersion in oil). The mixture was stirred for 15 minutes at the same temperature. To the reaction mixture was added 14.10 g (50 mmol) of phthalimide, which was stirred for 6 hours at 100° C. After cooling, the reaction mixture was then poured into water, extracted with chloroform. The extract solution was dried over anhydrous magnesium sulfate, the solvent was distilled off. The residue was purified by column chromatography (eluent: ethyl acetate) to give 11.43 g of the desired compound (61.1%, pale yellow solid).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06251905B1 |
| Source dataset | uspto-grants-2001_06 |
| ORD ID | ord-78fb24034fd94bbcbd582b6ff07f30cb |
| Source note | uspto-grants-2001_06 |