반응 #710478

ord-9eb9c378810042e192573892e1b2cbf6

반응 방정식

Nc1ccccn1
2-aminopyridine
CCN=C=NCCCN(C)C.Cl
EDC-HCl
O=C(O)C(F)(F)C(F)(F)F
pentafluoropropionic acid
O=C(N=c1cccc[nH]1)C(F)(F)C(F)(F)F
2,2,3,3,3-pentafluoro-N-(pyridin-2(1H)-ylidene)propanamide
수율 11.1%

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    세척washed once with water and twice with 1% hydrochloric acid
  2. 2
    건조dried over anhydrous magnesium sulfate
  3. 3
    농축concentrated under reduced pressure

실험 절차

300 mg (3.19 mmol) of 2-aminopyridine was dissolved in 15 ml of anhydrous dichloromethane, 919 mg (4.78 mmol) of EDC-HCl, 583 mg (4.78 mmol) of DMAP and 397 μl (628 mg, 3.83 mmol) of pentafluoropropionic acid were added thereto in sequence, and the resulting mixture was stirred at room temperature overnight. After the reaction was completed, the reaction solution was diluted with dichloromethane, washed once with water and twice with 1% hydrochloric acid, and then dried over anhydrous magnesium sulfate and concentrated under reduced pressure to obtain 85 mg (yield 11%) of 2,2,3,3,3-pentafluoro-N-(pyridin-2(1H)-ylidene)propanamide.

출처

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