HuagongsheHuagongshe Chemistry Print Report · For research reference only
Hydrochloric Acid → 2,5,6,7,8,9-Hexahydro-1′-methylspiro[3H-furo[2,3-h][1]benzazepine-3,4′-piperidine]
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Hydrochloric Acid | HCID 313 | — |
| Reactant | HCID 23225271 | HCID 23225271 | — |
| Product | 2,5,6,7,8,9-Hexahydro-1′-methylspiro[3H-furo[2,3-h][1]benzazepine-3,4′-piperidine] | HCID 21833851 | 90.9% |
Reaction Steps
5-Acetyl-3,5,6,7,8,9-hexahydro-1'-methylspiro [2H-furo[2,3-h]benzazepine-3,4'-piperidine] (D27, 0.25 g, 0.82 mmol) was stirred at reflux under Ar in c. HCl (15 ml) for 4 days. It was then evaporated to dryness, dissolved in dichloromethane, washed with K2CO3 solution, dried (Na2SO4) and evaporated to give the title compound (0.203 g) as a brown gum, still containing ca. 15% of amide (NMR). Chromatography on silica, eluting with 0-15% methanol in dichloromethane, give purer material (0.107 g, 49%)
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US05972951 |
| Source dataset | uspto-grants-1999_10 |
| ORD ID | ord-36a98028ef24419a8d74cef7adb7b7b6 |
| Source note | uspto-grants-1999_10 |