反応 #710475

ord-257a8f432d0c4ef5aa005a2342a2e2f5

反応方程式

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
収率 24.0%

反応条件

詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    洗浄washed with water and 1% hydrochloric acid
  2. 2
    乾燥dried over anhydrous magnesium sulfate

実験手順

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.

出典

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