Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Bromoacetonitrile → 4-(5-Chloro-2-hydroxy-phenyl)-4-oxo-butyronitrile
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Bromoacetonitrile | HCID 11534 | — |
| 반응물 | 3-Chloro-6-hydroxyacetophenone | HCID 74061 | — |
| 반응물 | Carbonic acid, monomethyl ester, magnesium salt (2:1) | HCID 167017 | — |
| 용매 | Hydrochloric Acid | HCID 313 | — |
| 생성물 | 4-(5-Chloro-2-hydroxy-phenyl)-4-oxo-butyronitrile | HCID 21973322 | 58.6% |
반응 단계
A solution of 1-(5-chloro-2-hydroxy-phenyl)-ethanone (1.0 g, 5.86 mmol) and magnesium methylcarbonate (13 mL, 32.5 mmol, 2.5 M solution in DMF) was stirred at 120° C. for 3 hours. The mixture was cooled to ambient temperature followed by the addition of bromoacetonitrile (1.22 mL, 17.6 mmol). The resulting solution was stirred at 90° C. for 3 hours. The reaction was cooled to ambient temperature then slowly poured into 1 M hydrochloric acid (200 mL). This was extracted with ethyl acetate, washed with brine, dried over magnesium sulfate, filtered and concentrated. Flash chromatography on silica gel gave the title compound (0.72 g).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US07098212B2 |
| 출처 데이터셋 | uspto-grants-2006_08 |
| ORD ID | ord-17531f7d84eb482b9d2cd0545ab98c03 |
| 출처 메모 | uspto-grants-2006_08 |