تفاعل #77417

ord-83e19880b15942178674c58a66ff69b7

ظروف التفاعل

الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    درجة الحرارةunder reflux for an additional 10 min
  2. 2
    درجة الحرارةThe mixture was cooled to 0° C.
  3. 3
    workup.STIRRINGThe mixture was stirred at 0° C. for several min
  4. 4
    ترشيحthe precipitate was filtered
  5. 5
    غسيلwashed several times with water
  6. 6
    تجفيفdried in vacuo over P2O5

الإجراء التجريبي

A suspension of 2-bromo-6-benzoylthioureidopyridine (4.99 g, 14.84 mmol) in 10% aqueous sodium hydroxide solution (10.4 mL, 26 mmol) was stirred at rt. for 10 min and then under reflux for an additional 10 min. The mixture was cooled to 0° C. and acidified with 1 N aqueous HCl solution to pH 4.0 and then adjusted to pH 8.5 with satd. aqueous potassium bicarbonate solution. The mixture was stirred at 0° C. for several min and the precipitate was filtered, washed several times with water and dried in vacuo over P2O5 to obtain the titled compound (3.23 g, 94%) as a white solid.

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US06706717B2uspto-grants-2004_03