Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Acetic Acid → 2-(4-Chlorobenzoyl)-3-methylhex-2-enenitrile
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Acetic Acid | HCID 176 | — |
| 반응물 | Beta-Alanine | HCID 239 | — |
| 반응물 | 2-Pentanone | HCID 7895 | — |
| 반응물 | 4-Chlorobenzoylacetonitrile | HCID 138308 | — |
| 용매 | Toluene | HCID 1140 | — |
| 용매 | Ethyl Acetate | HCID 8857 | — |
| 생성물 | 2-(4-Chlorobenzoyl)-3-methylhex-2-enenitrile | HCID 67054610 | — |
반응 단계
A mixture of pentan-2-one (20 mmol), 3-(4-chlorophenyl)-3-oxopropanenitrile (3.6 g, 20 mmol), β-alanine (180 mg, 2 mmol), acetic acid (2.6 mL) and toluene (60 mL) is heated to reflux in a Dean-Stark system for 18 h. The solution is cooled to RT, then diluted with EtOAc (50 mL), washed with 5% NaHCO3 (3×20 mL), water (20 mL), brine (20 mL), dried (Na2SO4) and finally concentrated in vacuo. A mixture of the two isomers is obtained as a colorless oil by chromatographic purification of the crude residue on silica gel using EtOAc:petroleum ether (0.5:9.5) as eluent.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US07897596B2 |
| 출처 데이터셋 | uspto-grants-2011_03 |
| ORD ID | ord-40d212c38f51454c9755e7e451e5617c |
| 출처 메모 | uspto-grants-2011_03 |