Reaktion #70124

ord-d932d86fdda44311868fb1815d018b40

Reaktionsgleichung

C=C(C)C(=O)Cl
methacrylic acid chloride
CCC1(O)CCC(C(F)(F)F)CC1
1-ethyl-4-trifluoromethylcyclohexanol
CCN(CC)CC
triethylamine
C=C(C)C(=O)OC1(CC)CCC(C(F)(F)F)CC1
1-ethyl-4-(trifluoromethyl)cyclohexyl methacrylate
Ausbeute 75.7%

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    SonstigeA four-necked flask equipped with a stirrer
  2. 2
    Sonstigeto obtain a solution
  3. 3
    SonstigeA solution prepared
  4. 4
    workup.ADDITIONwas added to the solution at 4° C. over 30 minutes
  5. 5
    workup.STIRRINGThe mixture was stirred at 4° C. for 3 hours
  6. 6
    Sonstigeto obtain a reaction mixture
  7. 7
    WaschenThe reaction mixture was washed with water

Vorschrift

A four-necked flask equipped with a stirrer, a thermometer, and a dropping funnel was charged with 7.9 g (0.04 mol) of 1-ethyl-4-trifluoromethylcyclohexanol, 0.2 g of 4-dimethylaminopyridine, 4.9 g of triethylamine, and 20 g of acetone. The mixture was stirred to obtain a solution. A solution prepared by dissolving 4.6 g (0.044 mol) of methacrylic acid chloride in 5 g of acetone was added to the solution at 4° C. over 30 minutes. The mixture was stirred at 4° C. for 3 hours to obtain a reaction mixture. The reaction mixture was washed with water to obtain 8.0 g of 1-ethyl-4-(trifluoromethyl)cyclohexyl methacrylate (hereinafter may be referred to as “compound (M-3)” ((M-3) in Table 1)). The yield of 1-ethyl-4-(trifluoromethyl)cyclohexyl methacrylate with respect to 1-ethyl-4-trifluoromethylcyclohexanol was 76%.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US08535871B2uspto-grants-2013_09