تفاعل #75109

ord-fdddbad9af684facba6a78d5104ad7e5

المذيبات

ظروف التفاعل

درجة الحرارة
-10°CELSIUS
الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    أخرىat 35° C
  2. 2
    workup.WAITleft
  3. 3
    workup.WAITto stand at 5° C. overnight
  4. 4
    ترشيحThe solid material is filtered off
  5. 5
    أخرىrecrystallized from ethanol, there

الإجراء التجريبي

75 G. of 2,4-diamino-6-chloropyrimidine are dissolved in 1500 ml. of ethanol at 35° C. The solution is cooled to -10° C. and a solution of 100 g. of 3-chloroperbenzoic acid in 500 ml. of ethanol is slowly added dropwise in the course of 1 hour. The suspension is subsequently stirred at -10° C. for 7 hours and left to stand at 5° C. overnight. The suspension is neutralized with 24 g. of sodium hydroxide in 100 ml. of water. The solid material is filtered off and recrystallized from ethanol, there being obtained pure 2,4-diamino-6-chloropyrimidine-3-oxide.

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US04175189uspto-grants-1979_11