تفاعل #6977

ord-55368fddc085434994f442da384179d4

الكواشف

لا شيء

المذيبات

ظروف التفاعل

درجة الحرارة
40°CELSIUS
الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    أخرىthe volatiles were removed in vacuo
  2. 2
    أخرىthe solid formed
  3. 3
    ترشيحwas collected by filtration
  4. 4
    غسيلrinsed with water
  5. 5
    أخرىdried

الإجراء التجريبي

A mixture of ethyl-6-amino-nicotinate (2.5 g, 15 mmol) and benzoyl isothiocyanate (2.45 g, 15 mmol) in THF (20 mL) was heated at 40° C. for 4 h. To this mixture at RT, was added sodium ethoxide (2.04 g, 30 mmol) in ethanol (10 mL). After stirring the resulting mixture at RT for 16 h, the volatiles were removed in vacuo. The residue was suspended in aqueous NH4Cl and the solid formed was collected by filtration, rinsed with water and dried to afford 6-thioureido-nicotinic acid ethyl ester as a white solid (2.6 g, 77% yield). LC/MS; (M+H)+=226.

المصدر

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