HuagongsheHuagongshe Chemistry Print Report · For research reference only
Hexane → HCID 21474126, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Hexane | HCID 8058 | — |
| Reactant | Sodium Hydroxide | HCID 14798 | — |
| Reactant | HCID 21474134 | HCID 21474134 | — |
| Solvent | Formic Acid | HCID 284 | — |
| Solvent | Formaldehyde | HCID 712 | — |
| Product | HCID 21474126 | HCID 21474126 | 76% |
Reaction Steps
Dissolved 3-(10,11-dihydro-5H-dibenzo[a,d]cyclohepten-5-yl)-piperidine (0.75 g, 2.7 mmol) in 1.1 mL of formic acid and 1.5 mL of 37% aqueous formaldehyde. Heated in a 90°-95° C. oil bath for 20 hours. Cooled to room temperature, and made basic with 5% NaOH. Extracted with ether. Dried combined organic extracts with MgSO4, filtered, and evaporated. Crystallized product from hexane to give 0.60 g (76% yield) of 3-(10,11-dihydro-5H-dibenzo[a,d]cyclohepten-5-yl)-1-methyl-piperidine as white solid. Dissolved the free base in ether, and added 19 weight % HCl-EtOH to precipitate the hydrochloride salt.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US05688805 |
| Source dataset | uspto-grants-1997_11 |
| ORD ID | ord-0096625f7a0643e29297fb1736e4373c |
| Source note | uspto-grants-1997_11 |