Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Pentyl nitrite → Piperidine, 1-methyl-4-phenoxy-4-phenyl-
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Pentyl nitrite | HCID 10026 | — |
| 반응물 | Piperidine, 4-(p-aminophenoxy)-1-methyl-4-phenyl- | HCID 3060392 | — |
| 용매 | Tetrahydrofuran | HCID 8028 | — |
| 생성물 | Piperidine, 1-methyl-4-phenoxy-4-phenyl- | HCID 3060394 | 26.2% |
반응 단계
A solution of 4-(4-aminophenoxy)-1-methyl-4-phenylpiperidine (2.82 g, 10 mM), in THF (75 ml) was added over 2 hours to a refluxing solution of amyl nitrite (2.7 ml, 20 mM) in THF (30 ml). After 5 hours at reflux amyl nitrite (1.5 ml) was added and the mixture maintained at reflux for 24 hours. The solvent was removed under reduced pressure and the residue partitioned between 2 N hydrochloric acid (50 ml) and ether (50 ml). The aqueous phase was basified (pH9) and extracted with ether (2×100 ml). The organic phase was dried and the solvents removed under reduced pressure. Sublimation of the residue at 1.0 mbar pressure (bath temp. 100°) gave the title compound (700 mg), m.p. 103°-4°.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US04325953 |
| 출처 데이터셋 | uspto-grants-1982_04 |
| ORD ID | ord-ec005ad339844366b79f7d9d4f6194ef |
| 출처 메모 | uspto-grants-1982_04 |