Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Diethyl Ether → 1-[(3,4-Dihydro-2-naphthalenyl)methyl]-4-(2-methoxyphenyl)piperazine
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Diethyl Ether | HCID 3283 | — |
| 반응물 | Sodium Bicarbonate | HCID 516892 | — |
| 반응물 | 1,2,3,4-Tetrahydro-2-[[4-(2-methoxyphenyl)-1-piperazinyl]methyl]-1-naphthalenol | HCID 22755562 | — |
| 용매 | Water | HCID 962 | — |
| 용매 | Acetic acid sulfuric acid | HCID 23350293 | — |
| 생성물 | 1-[(3,4-Dihydro-2-naphthalenyl)methyl]-4-(2-methoxyphenyl)piperazine | HCID 22755587 | 98.4% |
반응 단계
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.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US04130646 |
| 출처 데이터셋 | uspto-grants-1978_12 |
| ORD ID | ord-d2b273b9385a4b05a27f1ab9c1177119 |
| 출처 메모 | uspto-grants-1978_12 |