反応 #710489

ord-233d5483555847c5ab0ed247dba736f8

反応方程式

O=C(N=CCc1ncc(C(F)(F)F)cc1Cl)c1ccccc1C(F)(F)F
N-{2-[3-chloro-5-(trifluoromethyl)pyridin-2-yl]ethylidene}-2-(trifluoromethyl)benzamide
CC(=O)O
acetic acid
CC(=O)OC(Cc1ncc(C(F)(F)F)cc1Cl)NC(=O)c1ccccc1C(F)(F)F
desired product
収率 24.0%
CC(=O)OC(Cc1ncc(C(F)(F)F)cc1Cl)NC(=O)c1ccccc1C(F)(F)F
2-[3-chloro-5-(trifluoromethyl)pyridin-2-yl]-1-{[2-(trifluoromethyl)benzoyl]amino}ethyl acetate
収率 24.0%

反応条件

詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    温度heated to 90° C. for one day
  2. 2
    workup.WAITleft at room temperature for four days
  3. 3
    濃縮After concentration in vacuo
  4. 4
    その他the crude product was purified by chromatography on silica gel

実験手順

0.16 g of N-{2-[3-chloro-5-(trifluoromethyl)pyridin-2-yl]ethylidene}-2-(trifluoromethyl)benzamide (Int-6) were diluted in 2 mL of acetic acid. The reaction mixture was stirred for two days at room temperature and then heated to 90° C. for one day and left at room temperature for four days. After concentration in vacuo, the crude product was purified by chromatography on silica gel to yield 0.045 g (24%) of desired product 2-[3-chloro-5-(trifluoromethyl)pyridin-2-yl]-1-{[2-(trifluoromethyl)benzoyl]amino}ethyl acetate (Ia-112), [M+1]=455.

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US09301526B2uspto-grants-2016_04