Reaktion #710475

ord-257a8f432d0c4ef5aa005a2342a2e2f5

Reaktionsgleichung

Nc1ccccn1
2-aminopyridine
CCN=C=NCCCN(C)C.Cl
EDC-HCl
O=C(O)C(F)(F)Cl
chlorodifluoroacetic acid
O=C(N=c1cccc[nH]1)C(F)(F)Cl
2-chloro-2,2-difluoro-N-(pyridin-2(1H)-ylidene)acetamide
Ausbeute 24.0%

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Waschenwashed with water and 1% hydrochloric acid
  2. 2
    Trocknendried over anhydrous magnesium sulfate

Vorschrift

200 mg (2.13 mmol) of 2-aminopyridine was dissolved in 5 ml of dichloromethane, 491 mg (2.55 mmol) of EDC-HCl, 311 mg (2.55 mmol) of DMAP and 187 μl (2.23 mmol, 290 mg) of chlorodifluoroacetic acid were added thereto in sequence, and the resulting mixture was stirred overnight. After the reaction was completed, the reaction solution was diluted with dichloromethane, washed with water and 1% hydrochloric acid, and then dried over anhydrous magnesium sulfate to obtain 105 mg (yield 24%) of 2-chloro-2,2-difluoro-N-(pyridin-2(1H)-ylidene)acetamide.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US09301525B2uspto-grants-2016_04