반응 #710473

ord-bcb4421405d34698b8aef0a94d9dfd49

반응 방정식

O=C(O)C(F)F
difluoroacetic acid
CCN=C=NCCCN(C)C.Cl
EDC-HCl
Nc1ccccn1
2-aminopyridine
O=C(N=c1cccc[nH]1)C(F)F
2,2-difluoro-N-(pyridin-2(1H)-ylidene)acetamide
수율 14.0%

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    세척washed once with water and twice with a 1% HCl aqueous solution
  2. 2
    건조dried over anhydrous magnesium sulfate
  3. 3
    농축concentrated under reduced pressure

실험 절차

400 mg (4.26 mmol) of 2-aminopyridine was dissolved in 10 ml of anhydrous dichloromethane, 322 μl (490 mg, 5.11 mmol) of difluoroacetic acid, 982 mg (5.10 mmol) of EDC-HCl and 622 mg (5.11 mmol) of DMAP were added thereto, and the resulting mixture was stirred at room temperature for 61 hours. After the reaction was completed, the reaction solution was diluted with dichloromethane, washed once with water and twice with a 1% HCl aqueous solution, and then dried over anhydrous magnesium sulfate and concentrated under reduced pressure to obtain 102 mg (yield 14%) of 2,2-difluoro-N-(pyridin-2(1H)-ylidene)acetamide.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US09301525B2uspto-grants-2016_04