反应 #710478

ord-9eb9c378810042e192573892e1b2cbf6

反应方程式

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
收率 11.1%

反应条件

详细条件
See reaction.notes.procedure_details.

后处理

  1. 1
    洗涤washed once with water and twice with 1% hydrochloric acid
  2. 2
    干燥dried over anhydrous magnesium sulfate
  3. 3
    浓缩concentrated under reduced pressure

实验过程

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.

来源

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