Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
3-Nitrobenzaldehyde → Ethyl 4,4,4-trichloro-2-(3-nitrophenylmethylene)-3-oxobutanoate
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | 3-Nitrobenzaldehyde | HCID 7449 | — |
| 반응물 | Piperidine | HCID 8082 | — |
| 반응물 | Hexanoic Acid | HCID 8892 | — |
| 반응물 | Ethyl 4,4,4-trichloro-3-oxobutyrate | HCID 77294 | — |
| 용매 | Toluene | HCID 1140 | — |
| 생성물 | Ethyl 4,4,4-trichloro-2-(3-nitrophenylmethylene)-3-oxobutanoate | HCID 54196727 | 28.9% |
반응 단계
3-Nitrobenzaldehyde (7.55 g, 50 mmoles), ethyl 4,4,4-trichloro-3-oxobutanoate (18.33 g, 59.5 mmoles), piperidine (0.66 ml) and hexanoic acid (0.33 ml) were heated at reflux in toluene (130 ml) for 48 hours using a Dean and Stark apparatus. The mixture was cooled, evaporated to dryness in vacuo and crystallised by trituration with ethyl acetate/petroleum ether (60°-80°). Recrystallisation from 2-propanol gave the sub-title compound (5.3 g) mp 105.5°-7°.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US04607041 |
| 출처 데이터셋 | uspto-grants-1986_08 |
| ORD ID | ord-0f5d9b338d8f460eab0a9a6edb5f6d22 |
| 출처 메모 | uspto-grants-1986_08 |