Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Hydrazine, ethyl-, ethanedioate (1:1) → 4-(5-benzyl-1-ethyl-(1H-pyrazol-3-yl))-1-t-butoxycarbonylpiperidine
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Hydrazine, ethyl-, ethanedioate (1:1) | HCID 96181 | — |
| 반응물 | Tert-butyl 4-(3-oxo-4-phenylbutanoyl)piperidine-1-carboxylate | HCID 18187492 | — |
| 용매 | Methanol | HCID 887 | — |
| 생성물 | 4-(5-benzyl-1-ethyl-(1H-pyrazol-3-yl))-1-t-butoxycarbonylpiperidine | HCID 18187572 | — |
반응 단계
1-(1-(t-Butoxycarbonyl)piperidin-4-yl)-4-phenylbutane-1,3-dione from Step A, from Method A or Method B, Step B3, (0.851 g, 2.46 mmol) in methanol (25 mL) was added over 10 min to a suspension of ethylhydrazine oxalate (0.444 g, 2.96 mmol) in methanol (5 mL) in a 60° C. oil bath. After 15 h, the reaction was concentrated in vacuo and the residue was purified by repeated FC using a gradient of 50-100% ethyl acetate in hexanes to give first 4-(5-benzyl-1-ethyl-(1H)-pyrazol-3-yl)-1-(t-butoxycarbonyl)piperidine (0.148 g total) as the higher Rf product isomer and then the title compound (0.373 g total) as the lower Rf.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US06358979B1 |
| 출처 데이터셋 | uspto-grants-2002_03 |
| ORD ID | ord-aed7462254044a879c7c6e67b28059ee |
| 출처 메모 | uspto-grants-2002_03 |