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HRID 556246作成日:2026年10月26日

Sodium Iodide → Triphenylsulfonium 1,1,3,3,3-pentafluoro-2-(4-methacryloyloxy-butyryloxy)-propane-1-sulfonate

https://huagongshe.com/reaction/556246

反応式

関与物質

役割名称HCID仕込み量
反応物Sodium IodideHCID 5238—
反応物2,2'-Methylenebis(4-methyl-6-tert-butylphenol)HCID 8398—
反応物Sodium methacrylateHCID 3255932—
反応物Triphenylsulfonium 2-(4-chlorobutyryloxy)-1,1,3,3,3-pentafluoropropane-1-sulfonateHCID 86639509—
溶媒WaterHCID 962—
溶媒DimethylformamideHCID 6228—
溶媒DichloromethaneHCID 6344—
生成物Triphenylsulfonium 1,1,3,3,3-pentafluoro-2-(4-methacryloyloxy-butyryloxy)-propane-1-sulfonateHCID 86639511—

反応条件

温度90 °C

反応手順

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.

情報源と証拠

DOI10.6084/m9.figshare.5104873.v1
特許番号US08057985B2
出典データセットuspto-grants-2011_11
ORD IDord-7d4dbbd4c503453a849660fd9226dbcb
出典メモuspto-grants-2011_11