HuagongsheHuagongshe Chemistry Print Report · For research reference only
Diethyl Ether → 1-[(3,4-Dihydro-2-naphthalenyl)methyl]-4-(2-methoxyphenyl)piperazine
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Diethyl Ether | HCID 3283 | — |
| Reactant | Sodium Bicarbonate | HCID 516892 | — |
| Reactant | 1,2,3,4-Tetrahydro-2-[[4-(2-methoxyphenyl)-1-piperazinyl]methyl]-1-naphthalenol | HCID 22755562 | — |
| Solvent | Water | HCID 962 | — |
| Solvent | Acetic acid sulfuric acid | HCID 23350293 | — |
| Product | 1-[(3,4-Dihydro-2-naphthalenyl)methyl]-4-(2-methoxyphenyl)piperazine | HCID 22755587 | 98.4% |
Reaction Steps
6.0 g of 1,2,3,4-tetrahydro-2-[[4-(2-methoxyphenyl)-1-piperazinyl]methyl]-1-naphthalenol (prepared as described in Example 1) is suspended in 24 ml of 20% sulfuric acid/acetic acid and the mixture is heated on a steam bath for 15 minutes. The reaction mixture is then cooled room temperature, diluted with water (200 ml) and then made alkaline to pH 8 using sodium bicarbonate solution. The alkaline suspension is extracted with two 250 ml portions of methylene chloride and the organic phase is back-washed with water (250 ml), dried over anhydrous sodium sulfate, filtered and concentrated. The syrup obtained solidifies upon addition of a minimal amount of ether to yield 5.6 g of the title compound, melting point 84°-85° C.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US04130646 |
| Source dataset | uspto-grants-1978_12 |
| ORD ID | ord-d2b273b9385a4b05a27f1ab9c1177119 |
| Source note | uspto-grants-1978_12 |