反应 #1269822

反应方程式

sodium 2-[(methacryloyloxy)acetoxy]-1,1-difluoroethanesulfonate

water

triphenylsulfonium bromide

→

triphenylsulfonium 2-[(methacryloyloxy)acetoxy]-1,1-difluoroethanesulfonate

溶剂

chloroform

反应条件

后处理

1. 1
   workup.ADDITIONwere added
2. 2
   其他subjected to separation
3. 3
   洗涤The thus-obtained organic phase was washed with 15 mL of water
4. 4
   其他subjected to solvent evaporation

实验过程

Into a 200-mL reaction vessel, 5.77 g (purity: 44%, 8.56 mmol) of sodium 2-[(methacryloyloxy)acetoxy]-1,1-difluoroethanesulfonate obtained in Preparation Example 2-1, 15 mL of water and 15 mL of chloroform were added. Then, 2.9 g (8.6 mmol) of triphenylsulfonium bromide was dropped into the reaction vessel at room temperature. The resulting solution was stirred for 2 hours at room temperature and subjected to separation. The thus-obtained organic phase was washed with 15 mL of water and subjected to solvent evaporation, thereby obtaining 3.58 g of target triphenylsulfonium 2-[(methacryloyloxy)acetoxy]-1,1-difluoroethanesulfonate as a crude product. The purity of the crude target product was 57%; and the yield of the crude target product was 76%. The obtained crude triphenylsulfonium 2-[(methacryloyloxy)acetoxy]-1,1-difluoroethanesulfonate was admixed with 6 g of chloroform, 3 g of ethyl acetate and 1.5 g of diisopropyl ether and totally dissolved in the solvent by heating. The resulting solution was cooled in air, thereby precipitating a solid out of the solution. The precipitated solid was filtered out and dried. With this, 2.32 g of the target 2-[(methacryloyloxy)acetoxy]-1,1-difluoroethanesulfonate was obtained with a purity of 98%.

来源