تفاعل #1442518

ord-105cf9d98cf64dc2b15039a5b806cae9

المذيبات

ظروف التفاعل

درجة الحرارة
50°CELSIUS
الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    workup.ADDITIONDuring the addition
  2. 2
    درجة الحرارةThe mixture was refluxed for 3 h
  3. 3
    درجة الحرارةafter cooling
  4. 4
    workup.STIRRINGstirred for 1 h
  5. 5
    ترشيحthe product was filtered off
  6. 6
    غسيلwashed with water
  7. 7
    أخرىdried under reduced pressure

الإجراء التجريبي

With stirring, 80 ml of concentrated sulfuric acid were added dropwise to 138 g (0.57 mol) potassium 3-(4-chlorophenyl)-3-cyanoacrylate in 1.2 l of 88% strength formic acid. During the addition, the temperature increased to 50° C. The mixture was refluxed for 3 h and, after cooling, put into 10 l of ice-water and then stirred for 1 h, and the product was filtered off, washed with water and dried under reduced pressure. Yield: 86.0 g of m.p. 144-145° C.

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US06586369B1uspto-grants-2003_07