반응 #159386

ord-ab6d7f67b8be411aa66b359ec94e8dac

용매

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    온도the reaction mixture was heated
  2. 2
    온도to reflux for 4 h
  3. 3
    기타The solvent was then removed in vacuo
  4. 4
    세척washed with sat. Rochelle salt solution
  5. 5
    건조The organic phase was dried over sodium sulfate
  6. 6
    기타the solvent was removed in vacuo
  7. 7
    기타The product with the molecular weight of 221.27 (C11H11NO2S) was obtained in this way

실험 절차

Tin chloride (11.8 g) was added to a solution of 5-cyclopropylethynyl-3-nitrothiophene-2-carboxylic acid methyl ester (6.26 g) in ethanol (250 ml), and the reaction mixture was heated to reflux for 4 h. The solvent was then removed in vacuo, and the residue was taken up again in ethyl acetate and washed with sat. Rochelle salt solution. The organic phase was dried over sodium sulfate and the solvent was removed in vacuo. The product with the molecular weight of 221.27 (C11H11NO2S) was obtained in this way; MS (ESI): 222 (M+H+).

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US08828991B2uspto-grants-2014_09