HuagongsheHuagongshe Chemistry Print Report · For research reference only
Trifluoroacetic acid → HCID 23343663, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Trifluoroacetic acid | HCID 6422 | — |
| Reactant | Trifluoroacetic anhydride | HCID 9845 | — |
| Reactant | 3-Iodo-5-(1-methyl-4-piperidinyl)-5H-dibenzo[a,d]cyclohepten-5-ol | HCID 20316853 | — |
| Product | HCID 23343663 | HCID 23343663 | — |
Reaction Steps
A solution of 3.23 g. of 1-methyl-4-(3-iodo-5-hydroxy-5H-dibenzo[a,d]cyclohepten-5-yl)piperidine, 30 ml. of trifluoroacetic acid and 10 ml. of trifluoroacetic anhydride is refluxed for 6 hours. The solution is concentrated on a rotary evaporator and the residue is made basic with 5% sodium hydroxide solution. The oil that precipitates is extracted into ether, and this ether phase is washed with water, dried over magnesium sulfate, filtered, and the ether removed on a rotary evaporator. The residue is triturated with acetonitrile, collected and dried to give 2.36 g. of material. This material is recrystallized from ethyl acetate to give pure (±)-1-methyl-4-(3-iodo-5H-dibenzo[a,d]cyclohepten-5-ylidene)piperidine, m.p. 166°-170°.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US04031223 |
| Source dataset | uspto-grants-1977_06 |
| ORD ID | ord-0ac114b2b970480095cfd8962331bc99 |
| Source note | uspto-grants-1977_06 |