تفاعل #1561220

ord-9547a76e43dc488cb3b91aa3c4fac3aa

الكواشف

لا شيء

المذيبات

ظروف التفاعل

الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    درجة الحرارةthe mixture was heated
  2. 2
    أخرىwas removed
  3. 3
    درجة الحرارةcontinue refluxing for half an hour
  4. 4
    أخرىAfter most of solvent was removed
  5. 5
    ترشيحthe solid was filtered
  6. 6
    غسيلwashed with 20% ethanol aqueous solution
  7. 7
    أخرىdried

الإجراء التجريبي

Phenylguanidine carbonate (13.5 g, 100 mmol), β-keto esters (22.3 g, 120 mmol) and 120 mL of toluene were added to 250 mL of flask in sequence, the mixture was heated to reflux with a Dean Stark trap until all the water was removed, and continue refluxing for half an hour. After most of solvent was removed, the reaction solution was cooled to room temperature, the solid was filtered, washed with 20% ethanol aqueous solution and dried to obtain 18.3 g of white solid (II-1) with yield of 71.2%.

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US09018218B2uspto-grants-2015_04