تفاعل #159386

ord-ab6d7f67b8be411aa66b359ec94e8dac

المذيبات

ظروف التفاعل

الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    درجة الحرارةthe reaction mixture was heated
  2. 2
    درجة الحرارةto reflux for 4 h
  3. 3
    أخرىThe solvent was then removed in vacuo
  4. 4
    غسيلwashed with sat. Rochelle salt solution
  5. 5
    تجفيفThe organic phase was dried over sodium sulfate
  6. 6
    أخرىthe solvent was removed in vacuo
  7. 7
    أخرىThe product with the molecular weight of 221.27 (C11H11NO2S) was obtained in this way

الإجراء التجريبي

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+).

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US08828991B2uspto-grants-2014_09