HuagongsheHuagongshe Chemistry Print Report · For research reference only
Ethanol → HCID 11719403, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Ethanol | HCID 702 | — |
| Reactant | Sulfuric Acid | HCID 1118 | — |
| Reactant | 859217-52-0 | HCID 11302685 | — |
| Solvent | Ethyl Acetate | HCID 8857 | — |
| Product | HCID 11719403 | HCID 11719403 | 96.1% |
Reaction Steps
To 1-cyclopropylmethyl-4-[2-(3,3,5,5-tetramethylcyclohexyl)phenyl]piperazine (300 mg, 0.846 mmol) were added ethyl alcohol (2.5 mL), 97% sulfuric acid (85.5 mg, 0.846 mmol) and ethyl acetate to form a thoroughly dissolved sate, and the mixture was slowly concentrated to dryness while adjusting reduced pressure. Diethyl ether was added thereto, and the solid was triturated by sonication. Precipitated crystals were collected by filtration, washed with diethyl ether, and aircured by aspiration. Drying under reduced pressure using a vacuum pump at room temperature gave 368 mg of the title compound as colorless crystals (crystal a).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07910734B2 |
| Source dataset | uspto-grants-2011_03 |
| ORD ID | ord-f5d15637786d4b3cb5ba93009226a45b |
| Source note | uspto-grants-2011_03 |