HuagongsheHuagongshe Chemistry Print Report · For research reference only
HCID 70896218, compound → HCID 70896188, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | HCID 70896218 | HCID 70896218 | — |
| Solvent | Methanol | HCID 887 | — |
| Solvent | Trifluoroacetic acid | HCID 6422 | — |
| Product | HCID 70896188 | HCID 70896188 | 88.4% |
Reaction Steps
A solution of 2-(4-methoxybenzyl)-7-(quinuclidin-3-ylmethyl)-8,9-dihydro-2H-azepino[5,4,3-cd]indazol-6(7H)-one (219 mg, 0.51 mmol) in trifluoroacetic acid (3 mL) was subjected to microwave irradiation at 130° C. for 18 min. The mixture was diluted with methanol and concentrated in vacuo. The resulting residue was converted to the free base by elution through an SCX-2 cartridge and then purified by column chromatography (silica gel, (12%-100% solvent mixture B in methylene chloride; solvent mixture B=70:27:3 methylene chloride/methanol/concentrated ammonium hydroxide) to afford 7-(quinuclidin-3-ylmethyl)-8,9-dihydro-2H-azepino[5,4,3-cd]indazol-6(7H)-one (140 mg, 88%) as a colorless oil: MS (ESI+) m/z 311 (M+H).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09045501B2 |
| Source dataset | uspto-grants-2015_06 |
| ORD ID | ord-92dcd5e1d9b54bad8fb529cb22c91658 |
| Source note | uspto-grants-2015_06 |