تفاعل #6973

ord-446464081e0447db9f4ca083cb4217ae

الكواشف

لا شيء

المذيبات

ظروف التفاعل

الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    تركيزThe mixture was concentrated to thin slurry and methanol
  2. 2
    workup.ADDITIONwas added
  3. 3
    ترشيحThe solid was filtered
  4. 4
    غسيلwashed with methanol
  5. 5
    أخرىdried

الإجراء التجريبي

A solution of ethyl 6-amino-nicotinate (830 mg, 5 mmol) and benzoyl isothiocyanate (830 mg, 5.1 mmol) in acetone was refluxed for 2 h. The mixture was concentrated to thin slurry and methanol was added. The solid was filtered, washed with methanol and dried to afford ethyl 6-(3-benzoyl-thioureido)-nicotinate (1.35 g, 82%). 1H NMR (CDCl3) δ 13.34 (s, 1 H), 9.04 (m, 3 H), 8.38 (s, 1 H), 7.93 (m, 2 H), 7.66 (m, 3 H), 4.42 (q, 2 H, J=7.6 Hz), 1.41(t, 3 H, J=7.6 Hz).

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US07084160B2uspto-grants-2006_08