반응 #303789

ord-2b0a786148ad47b296e6e9cc67051798

반응 방정식

CCN(CC)CC
Triethylamine
CCOC(=O)C(F)(F)Br
ethyl 2-bromo-2,2-difluoroacetate
N#Cc1ccc(-n2ccnc2S)c2ccccc12
4-(2-mercapto-1H-imidazol-1-yl)-1-naphthonitrile
CCOC(=O)C(F)(F)Sc1nccn1-c1ccc(C#N)c2ccccc12
ethyl 2-(1-(4-cyanonaphthalen-1-yl)-1H-imidazol-2-ylthio)-2,2-difluoroacetate

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    기타prepared
  2. 2
    세척The mixture was washed with aqueous HCl solution (0.2M), 50% saturated sodium chloride solution
  3. 3
    건조dried over sodium sulfate
  4. 4
    여과filtered
  5. 5
    농축concentrated
  6. 6
    workup.ADDITIONHexanes were added
  7. 7
    농축the mixture concentrated

실험 절차

Triethylamine (1.1 eq), followed by ethyl 2-bromo-2,2-difluoroacetate (1.05 eq) were added to a stirring slurry of 4-(2-mercapto-1H-imidazol-1-yl)-1-naphthonitrile (prepared as described herein, 1 eq) in dichloromethane and stirring continued for 3 h. The mixture was washed with aqueous HCl solution (0.2M), 50% saturated sodium chloride solution, dried over sodium sulfate, filtered, and concentrated. Hexanes were added and the mixture concentrated to provide ethyl 2-(1-(4-cyanonaphthalen-1-yl)-1H-imidazol-2-ylthio)-2,2-difluoroacetate.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US08193234B2uspto-grants-2012_06