반응 #1583807
ord-2559aebc93ea47b19234463dba5e3caa
반응 방정식
lithium bis(trimethylsilyl)amide
4-methylpyridine
ethyl 5-chlorothiophene-2-carboxylate
→
1-(5-Chloro-2-thienyl)-2-(pyridin-4-yl)ethanone
시약
없음
반응 조건
온도
5°CELSIUS
상세 조건
See reaction.notes.procedure_details.
후처리
- 1여과The resulting precipitate was filtered off
- 2여과filtered again
- 3기타dried
실험 절차
At 0° C., 64.5 ml of a 1M solution of lithium bis(trimethylsilyl)amide in hexane are added dropwise to a solution of 3.00 g (32.3 mmol) of 4-methylpyridine and 6.77 g (35.5 mmol) of ethyl 5-chlorothiophene-2-carboxylate in 58 ml THF, and the reaction mixture is stirred at 5° C. for 3 h. The resulting precipitate was filtered off, acidified with 6M HCl, filtered again and dried. This gives 2.9 g (35%) of the desired product; 1H-NMR (DMSO-d6): δ=8.53 (d, 2H), 8.09 (d, 1H), 7.40 (d, 1H), 7.34 (d, 2H), 4.39 (s, 2H).