تفاعل #1106

ord-ed5d30e63cae482aa9ed8a44a63361f9

معادلة التفاعل

COc1c(Cl)ccnc1C
4-chloro-3-methoxy-2-methylpyridine
CC(C)(C)c1ccc(N)cc1
4-tert-butylaniline
[Na+].[OH-]
NaOH
COc1c(Nc2ccc(C(C)(C)C)cc2)ccnc1C
4-(4-tert-Butylanilino)-3-methoxy-2-methylpyridine

الكواشف

لا شيء

المذيبات

ظروف التفاعل

الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    درجة الحرارةAfter cooling
  2. 2
    استخلاصthe product is extracted
  3. 3
    تركيزAfter concentrating
  4. 4
    workup.DISTILLATIONthe excess of amine is distilled off in vacuo
  5. 5
    أخرىthe residue is crystallized

الإجراء التجريبي

7.9 g of 4-chloro-3-methoxy-2-methylpyridine and 22.4 g of 4-tert-butylaniline are heated at 120° C. for 8 hours in 20 g of phenol. After cooling, the mixture is poured into NaOH and the product is extracted using methylene chloride. After concentrating, the excess of amine is distilled off in vacuo and the residue is crystallized using hexane. 9.5 g=55%

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US05723450uspto-grants-1998_03