Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Ethanol → Ethyl 3-bromoisonicotinate
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Ethanol | HCID 702 | — |
| 반응물 | Sulfuric Acid | HCID 1118 | — |
| 반응물 | 3-Bromoisonicotinic acid | HCID 817972 | — |
| 생성물 | Ethyl 3-bromoisonicotinate | HCID 15141565 | — |
반응 단계
3-bromoisonicotinic acid (3.0 g, 14.9 mmol) in ethanol (100 mL) was treated with concentrated sulfuric acid (5 mL). The mixture was brought to reflux at which time everything went into solution. After 12 hours at reflux, LCMS indicated that the reaction was complete. The reaction mixture was cooled to room temperature and concentrated on a rotary evaporator to a third of its original volume. The mixture was then diluted with 250 mL of ethyl acetate and washed twice with saturated aqueous sodium bicarbonate. Concentration on a rotary evaporator yielded 3.25 g of ethyl 3-bromoisonicotinate as a yellowish oil which was sufficiently pure enough for subsequent chemical transformations. LCMS (ESI) 216.2 (M+1)+.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US08853235B2 |
| 출처 데이터셋 | uspto-grants-2014_10 |
| ORD ID | ord-f6abebb8bb814cdea903f1325c22c9c0 |
| 출처 메모 | uspto-grants-2014_10 |