참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Ethanol | HCID 702 | — |
| 반응물 | Acetic Anhydride | HCID 7918 | — |
| 반응물 | Acetylacetone | HCID 31261 | — |
| 반응물 | Ethylorthoformate | HCID 53630039 | — |
| 용매 | Ethyl Acetate | HCID 8857 | — |
| 생성물 | 3-(Ethoxymethylene)pentane-2,4-dione | HCID 240418 | 17% |
반응 단계
A solution of Acetylacetone (40 mL), Ethyl orthoformate (95.4 mL) and Acetic anhydride (54.2 mL) was heated to reflux (150° C.) for 1 hour. The reaction solution was cooled to room temperature and was directly subjected to flash column chromatography (E. Merck Silica Gel (˜120 g); Eluent: 100% EtOAc followed by 5% EtOH in EtOAc). Concentration of the fractions containing the pure product using a rotavap at 40° C. afforded the title compound as a dark red viscous oil (10.4 g, 17.0%).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 특허 번호 | US09446046B2 |
|---|
| 출처 데이터셋 | uspto-grants-2016_09 |
|---|
| ORD ID | ord-2aa6503ec8d54b4c92015055e89bae7a |
|---|
| 출처 메모 | uspto-grants-2016_09 |
|---|
