反応 #710478

ord-9eb9c378810042e192573892e1b2cbf6

反応方程式

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
収率 11.1%

反応条件

詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    洗浄washed once with water and twice with 1% hydrochloric acid
  2. 2
    乾燥dried over anhydrous magnesium sulfate
  3. 3
    濃縮concentrated under reduced pressure

実験手順

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.

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US09301525B2uspto-grants-2016_04