반응 #1583807

ord-2559aebc93ea47b19234463dba5e3caa

반응 방정식

C[Si](C)(C)[N-][Si](C)(C)C.[Li+]
lithium bis(trimethylsilyl)amide
Cc1ccncc1
4-methylpyridine
CCOC(=O)c1ccc(Cl)s1
ethyl 5-chlorothiophene-2-carboxylate
O=C(Cc1ccncc1)c1ccc(Cl)s1
1-(5-Chloro-2-thienyl)-2-(pyridin-4-yl)ethanone

용매

반응 조건

온도
5°CELSIUS
상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    여과The resulting precipitate was filtered off
  2. 2
    여과filtered again
  3. 3
    기타dried

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).

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US09198426B2uspto-grants-2015_12