Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
1-Butanaminium, N,N,N-tributyl-, azide → HCID 86641873, 화합물
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | 1-Butanaminium, N,N,N-tributyl-, azide | HCID 5743232 | — |
| 반응물 | 1-(6-Fluoro-4-iodo-pyridin-3-yl)-ethanol | HCID 66738096 | — |
| 용매 | Dichloromethane | HCID 6344 | — |
| 생성물 | HCID 86641873 | HCID 86641873 | 78% |
반응 단계
Add tetra-N-butylammonium azide to a solution of triphenylphine (11 g, 42 mmol) and 1,4-cyclohexadiene-2,2-dicarbonitrile,4,5-dichloro-3,6-dioxo-(9 g, 40 mmol) in dichloromethane (150 mL) under ice-bath cooling. Then add 1-(6-fluoro-4-iodo-pyridin-3-yl)-ethanol (6.7 g, 25.1 mmol) to the above solution. Stir the mixture at room temperature for 1 hour. Concentrate the mixture in vacuo to about 50 mL. Purify the residue by flash column chromatography (hexane to 20% ethyl acetate in hexane as gradient) to give target product as colorless oil (5.7 g, 78%). MS (ES) m/z 293 [M+1]+.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US08063212B2 |
| 출처 데이터셋 | uspto-grants-2011_11 |
| ORD ID | ord-ca10d2d06b1b47eca7dfca38dbf2c0ce |
| 출처 메모 | uspto-grants-2011_11 |