HuagongsheHuagongshe Chemistry Print Report · For research reference only
Chlorosuccinimide → HCID 13457727, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Chlorosuccinimide | HCID 31398 | — |
| Reactant | HCID 13457725 | HCID 13457725 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | HCID 13457727 | HCID 13457727 | 55.7% |
Reaction Steps
A solution containing 5-(2-fluorophenyl)-1-methyl-1H-pyrrolo[1,2-b][1,2,5]triazepin-2(3H)-one hydrochloride (3.3 g, 12.9 mmol) and N-chlorosuccinimide (1.87 g, 14 mmol) in 100 ml of dry tetrahydrofuran was refluxed under N2 for 3 hours. The resultant solution was evaporated and the residual oil was taken up in 200 ml of EtOAc, washed with H2O, dried (MgSO4), filtered, and evaporated to an oil. This oil was purified by flash chromatography (silica, 4:7 hexane-ether) to given an oil (2.1 g). This oil was treated with ethereal HCl and the resultant solid was recrystallized from isopropanol-ether to give 2.36 g (55%) of powder, m.p. 218° dec.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US04517195 |
| Source dataset | uspto-grants-1985_05 |
| ORD ID | ord-e2dc9bd7c9af44659fc1b7b4ee933eb0 |
| Source note | uspto-grants-1985_05 |