تفاعل #54684

ord-1994be71994a4b1b94039e3c46ef7df0

معادلة التفاعل

CCO
ethanol
Nc1cc(Cl)nc(N)n1
2,4-diamino-6-chloropyrimidine
CCO
ethanol
[Na+].[OH-]
sodium hydroxide
O=C(OO)c1cccc(Cl)c1
3-chloroperbenzoic acid
Nc1cc(Cl)nc(N)[n+]1[O-]
2,4-diamino-6-chloropyrimidine-3-oxide

المذيبات

ظروف التفاعل

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

المعالجة

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

الإجراء التجريبي

75 G. of 2,4-diamino-6-chloropyrimidine are dissolved at 35° C. in 1500 ml. of ethanol. 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 within 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: US04150131uspto-grants-1979_04