HuagongsheHuagongshe Chemistry Print Report · For research reference only
Benzoyl chloride → HCID 46843286, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Benzoyl chloride | HCID 7412 | — |
| Reactant | Diisopropylethylamine | HCID 81531 | — |
| Reactant | Ether hydrochloride | HCID 10953452 | — |
| Reactant | HCID 66677239 | HCID 66677239 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | HCID 46843286 | HCID 46843286 | 79% |
Reaction Steps
3-Chloro-6,7,8,9-tetrahydro-5H-dipyrido[2,3-b;3′,4′-d]pyrrole (50 mg, 0.24 mmol) and DIEA (0.05 mL, 0.29 mmol) were dissolved in THF (2 ml). Benzoyl chloride (0.03 ml, 0.29 mmol) was added dropwise and the reaction was stirred at room temperature for 1 h. The crude reaction mixture was concentrated, and converted to the HCl salt by dissolving the crude material in MeOH (2 ml) and adding 1 M HCl/ether (2 equiv). The resulting solution was refrigerated overnight. The resulting precipitate was filtered and dried under vacuum to provide 19 (33 mg, 40% yield) as a pale yellow solid. LC-MS (M+H=312, obsd.=312).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08853391B2 |
| Source dataset | uspto-grants-2014_10 |
| ORD ID | ord-b4f504b2052b49d9b892e7e1e22f8332 |
| Source note | uspto-grants-2014_10 |