Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Hydrochloric Acid → 6-Bromo-2-methyl-2-(trifluoromethyl)chroman-4-one
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Hydrochloric Acid | HCID 313 | — |
| 반응물 | Malonic Acid | HCID 867 | — |
| 반응물 | Water | HCID 962 | — |
| 반응물 | Water ethanol | HCID 19096565 | — |
| 반응물 | HCID 178506234 | HCID 178506234 | — |
| 용매 | 1,4-Dioxane | HCID 31275 | — |
| 생성물 | 6-Bromo-2-methyl-2-(trifluoromethyl)chroman-4-one | HCID 67305602 | — |
반응 단계
A mixture of malonic acid (1.2 ml, 19 mmol) and (Z)-N-(6-bromo-2-(trifluoromethyl)-4H-chromen-4-ylidene)(phenyl)methanamine (6.63 g, 17 mmol) in dioxane was heated to reflux for 18 h until the reaction was completed. The mixture was cooled to RT and treated with 50% EtOH/H2O (20 ml) followed by conc. HCl (5.0 ml). The resulted mixture was left to stand at RT for 40 min, and then diluted with water (500 ml). The product was extracted with hexane (3×300 ml). The organic layers were combined, dried over Na2SO4, filtered and concentrated. The residue was purified on silica gel column (2-10% EtOAc/hexane) to afford the title compound as yellow oil. MS m/z: 310 (M+1).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US07745484B2 |
| 출처 데이터셋 | uspto-grants-2010_06 |
| ORD ID | ord-c3a2be2fa62a4184bb7028072a2a91f8 |
| 출처 메모 | uspto-grants-2010_06 |