HuagongsheHuagongshe Chemistry Print Report · For research reference only
Hydrochloric Acid → HCID 12412215, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Hydrochloric Acid | HCID 313 | — |
| Reactant | Sodium Hydroxide | HCID 14798 | — |
| Reactant | HCID 12412205 | HCID 12412205 | — |
| Solvent | Ethanol | HCID 702 | — |
| Product | HCID 12412215 | HCID 12412215 | 7.3% |
Reaction Steps
At 50° C, a solution comprising 18.25 g. (0.06 mole) of 1,1-dichloro-1a,10b-dihydrodibenzo(b,f)cycloprop(d)azepine-6(1H)-carboxaldehyde, 16.8 g. (0.42 mole) of sodium hydroxide and 319 g. of ethanol is stirred for 4.5 hours and, then, the reaction mixture is neutralized with conc. HCl. Ethanol is distilled off, water is added and extracted with ethyl acetate. The ethyl acetate extract is washed with water and dried with anhydrous sodium sulfate, followed by the distillation of the solventto dry up under reduced pressure. The residue is then recrystallized from benzene to give 12.0 g. (yield 7.30 %) of 1,1-dichloro-1,1a,6,10b-tetrahydrodibenzo(b,f)cycloprop(d)azepine. Meltingpoint: 162°-163° C
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US03992370 |
| Source dataset | uspto-grants-1976_11 |
| ORD ID | ord-0316ea867cd849ce855a4eefb305066e |
| Source note | uspto-grants-1976_11 |