تفاعل #710476

ord-03c4d64fd69f4a72b3916c9c53297123

معادلة التفاعل

ClCc1ccc(Cl)nc1
2-chloro-5-chloromethyl pyridine
O=C(N=c1cccc[nH]1)C(F)(F)Cl
2-chloro-2,2-difluoro-N-(pyridin-2(1H)-ylidene)acetamide
O=C([O-])[O-].[K+].[K+]
potassium carbonate
O=C(N=c1ccccn1Cc1ccc(Cl)nc1)C(F)(F)Cl
2-chloro-N-[1-((6-chloropyridin-3-yl)methyl)pyridin-2(1H)-ylidene]-2,2-difluoroacetamide

المذيبات

ظروف التفاعل

الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    أخرىsynthesized by the aforementioned method
  2. 2
    درجة الحرارةthe resulting mixture was heated
  3. 3
    درجة الحرارةrefluxed for 1 hours
  4. 4
    أخرىwas returned to room temperature
  5. 5
    تركيزconcentrated under reduced pressure
  6. 6
    workup.ADDITIONDiethyl ether was added
  7. 7
    أخرىto precipitate a solid
  8. 8
    أخرىthus the solid was collected
  9. 9
    أخرىdried
  10. 10
    أخرىto obtain the subject material
  11. 11
    أخرىAmount obtained 49 mg (yield 45%)

الإجراء التجريبي

53 mg (0.33 mmol) of 2-chloro-5-chloromethyl pyridine dissolved in 6 ml of anhydrous acetonitrile was added to 68 mg (0.33 mmol) of the 2-chloro-2,2-difluoro-N-(pyridin-2(1H)-ylidene)acetamide synthesized by the aforementioned method, and subsequently, 50 mg (0.36 mmol) of potassium carbonate was added thereto and the resulting mixture was heated and refluxed for 1 hours. After the reaction was completed, the reaction solution was returned to room temperature and then concentrated under reduced pressure. Diethyl ether was added thereto to precipitate a solid, and thus the solid was collected and dried to obtain the subject material. Amount obtained 49 mg (yield 45%).

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US09301525B2uspto-grants-2016_04