참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Nefazodone | HCID 4449 | — |
| 반응물 | Benzene, (2-bromoethoxy)- | HCID 68526 | — |
| 반응물 | Sodium | HCID 5360545 | — |
| 용매 | O-Xylene | HCID 7237 | — |
| 생성물 | Nefazodone Hydrochloride | HCID 54911 | 30.7% |
반응 단계
The sodium salt is pulverized, suspended in 200 ml. of xylene and mixed with phenoxyethyl bromide (10.4 g., 0.052 mole) in 20 ml. of xylene. The resulting mixture is refluxed with stirring for a 64 hr. period and the hot reaction mixture filtered. The filtrate is concentrated under reduced pressure and residual material taken up in ether. Insolubles are collected and the ether filtrate concentrated to afford 22.9 g. (94%) of 2-[3-[4-(3-chlorophenyl)-1-piperazinyl]propyl]-5-ethyl-4-(2-phenoxyethyl)-2H-1,2,4-triazol-3(4H)-one as the free base. Purification of the product is carried out by acidifying a solution of the free base in ethanol with ethanolic hydrogen chloride, and crystallization to afford hydrated (0.25 mole) 2-[3-[4-(3-chlorophenyl)-1-piperazinyl]propyl]-5-ethyl-4-(2-phenoxyethyl)-2H-1,2,4-triazol-3(4H)-one hydrochloride, m.p. 175°-177° C. (30.7% yield).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US04575555 |
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| 출처 데이터셋 | uspto-grants-1986_03 |
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| ORD ID | ord-b87a59b3c9564f8aacedc74b1ae53c34 |
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| 출처 메모 | uspto-grants-1986_03 |
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