反応 #1583807

反応方程式

lithium bis(trimethylsilyl)amide

4-methylpyridine

ethyl 5-chlorothiophene-2-carboxylate

→

1-(5-Chloro-2-thienyl)-2-(pyridin-4-yl)ethanone

溶媒

hexane

THF

反応条件

後処理

1. 1
   ろ過The resulting precipitate was filtered off
2. 2
   ろ過filtered again
3. 3
   その他dried

実験手順

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).

出典