تفاعل #68994

ord-401742739efe4f8dbe8bad0c9f5cf879

الكواشف

لا شيء

المذيبات

ظروف التفاعل

درجة الحرارة
0°CELSIUS
الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    workup.ADDITIONaddition
  2. 2
    درجة الحرارةto warm to room temperature
  3. 3
    ترشيحwas collected by filtration
  4. 4
    غسيلThe collected solids were washed with additional water
  5. 5
    أخرىbefore drying overnight in vacuo

الإجراء التجريبي

4-Methoxy-benzoyl chloride (4.15 mL, 30.7 mmol) was added dropwise to a stirred, cooled 0° C. mixture of 2,6-dichloro-pyridin-3-ylamine (5 g, 30.7 mmol) in pyridine (31 mL). Following addition, the reaction mixture was allowed to warm to room temperature and stirring was continued for 30 minutes, at which point the reaction mixture was poured into water causing the formation of a precipitate which was collected by filtration. The collected solids were washed with additional water before drying overnight in vacuo affording N-(2,6-dichloro-pyridin-3-yl)-4-methoxy-benzamide (8.66 g, 29.1 mmol, 95% yield) which was used in subsequent reactions without further purification. ES MS (M+H+)=297.

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US08530483B2uspto-grants-2013_09