반응 #643428

반응 방정식

sodium methacrylate

sodium iodide

2,2′-methylenebis(6-t-butyl-p-cresol)

triphenylsulfonium 2-(4-chlorobutyryloxy)-1,1,3,3,3-pentafluoropropane-1-sulfonate

→

triphenylsulfonium 1,1,3,3,3-pentafluoro-2-(4-methacryloyloxy-butyryloxy)-propane-1-sulfonate

용매

dimethylformamide

dichloromethane

water

반응 조건

후처리

1. 1
   온도The mixture was heated
2. 2
   기타to resume room temperature
3. 3
   기타The organic layer was separated
4. 4
   세척washed with water whereupon dichloromethane
5. 5
   workup.DISTILLATIONwas distilled off under vacuum
6. 6
   세척washed with water whereupon methyl isobutyl ketone
7. 7
   workup.DISTILLATIONwas distilled off under vacuum
8. 8
   기타The residue was purified by silica gel chromatography

실험 절차

To 20 g of dimethylformamide were added 5.4 g (9.0 mmol) of triphenylsulfonium 2-(4-chlorobutyryloxy)-1,1,3,3,3-pentafluoropropane-1-sulfonate synthesized in Synthesis Example 1-20, 1.2 g (11 mmol) of sodium methacrylate, 0.20 g (1.4 mmol) of sodium iodide, and 1 mg of 2,2′-methylenebis(6-t-butyl-p-cresol). The mixture was heated and stirred at 90° C. for 12 hours. The reaction solution was allowed to resume room temperature, after which 50 g of water and 80 g of dichloromethane were added. The organic layer was separated and washed with water whereupon dichloromethane was distilled off under vacuum. The residue was combined with 30 g of methyl isobutyl ketone and washed with water whereupon methyl isobutyl ketone was distilled off under vacuum. The residue was purified by silica gel chromatography. The target compound, triphenylsulfonium 1,1,3,3,3-pentafluoro-2-(4-methacryloyloxy-butyryloxy)-propane-1-sulfonate was obtained as brown oil (4.2 g, yield 72%). The compound has the following structure.

출처