Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Hydrochloric Acid → 1-(5-Chloropyridin-2-yl)ethan-1-one
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Hydrochloric Acid | HCID 313 | — |
| 반응물 | Dimethylacetamide | HCID 31374 | — |
| 반응물 | 2-Bromo-5-chloropyridine | HCID 817098 | — |
| 반응물 | Butyllithium | HCID 178418339 | — |
| 용매 | Water | HCID 962 | — |
| 용매 | Diethyl Ether | HCID 3283 | — |
| 용매 | Tetrahydrofuran | HCID 8028 | — |
| 생성물 | 1-(5-Chloropyridin-2-yl)ethan-1-one | HCID 10154166 | — |
반응 단계
To a suspension of 56 g of 2-bromo-5-chloropyridine in 560 ml of dry diethylether is added a solution of 179 ml of n-butyllithium (15% solution in hexane) at -78° and under argon at such a rate that the temperature never exceeds -72°. Immediately thereafter the solution of 25.7 ml of N,N-dimethylacetamide in dry THF is added. The mixture is stirred for one hour at the same temperature and thereafter decomposed by careful addition of 100 ml of 3N hydrochloric acid, followed by 100 ml of water with vigorous cooling. Working up by process A (see Example 1) and purification by chromatogrphy over silica gel (toluene/ethyl acetate=20/1) yields the compound as white needles; m.p.: 58°-65°.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US05622982 |
| 출처 데이터셋 | uspto-grants-1997_04 |
| ORD ID | ord-7dc9fd34c3da4470aeca855928a96ee5 |
| 출처 메모 | uspto-grants-1997_04 |