HuagongsheHuagongshe Chemistry Print Report · For research reference only
Trichloroacetyl chloride → 2,2,2-Trichloro-1-[10-(9H-fluorene-2-carbonyl)-10,11-dihydro-5H-pyrrolo[2,1-c][1,4]benzodiazepin-3-yl]-ethanone
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Trichloroacetyl chloride | HCID 6420 | — |
| Reactant | 10-(9H-Fluoren-2-ylcarbonyl)-10,11-dihydro-5H-pyrrolo[2,1-c][1,4]benzodiazepine | HCID 68690693 | — |
| Solvent | 1,4-Dioxane | HCID 31275 | — |
| Product | 2,2,2-Trichloro-1-[10-(9H-fluorene-2-carbonyl)-10,11-dihydro-5H-pyrrolo[2,1-c][1,4]benzodiazepin-3-yl]-ethanone | HCID 68686423 | 88.6% |
Reaction Steps
To 25 mL of 1,4-dioxane was added 0.59 g (0.0016 mol) of 10-(9H-fluoren-2-ylcarbonyl)-10,11-dihydro-5H-pyrrolo[2,1-c][1,4]benzodiazepine opf Step A followed by the addition of 0.31 g (0.0017 mol) of trichloroacetyl chloride. The solution was heated under reflux for 10 minutes, cooled to room temperature and poured into ice water with stirring The precipitate was collected, washed with water and dried yielding 0.74 g of title compound which was used directly in the next step.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07678787B2 |
| Source dataset | uspto-grants-2010_03 |
| ORD ID | ord-8a607f0b468f42d086b8e5b8b9bbd66c |
| Source note | uspto-grants-2010_03 |