Fluorine-containing sulfonates having polymerizable anions and manufacturing method therefor, fluorine-containing resins, resist compositions, and pattern-forming method using same
A kind of polymerization and sulfonate technology, which is applied in the preparation of sulfonate, the application of radioactive source radiation, the photoplate making process of pattern surface, etc., which can solve the problems of expensive sulfonic acid and so on
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[0318] Hereinafter, the present invention will be described in detail using synthesis examples, examples, and reference examples, but the present invention is not limited to the following examples.
[0319] First, two types of polymerizable monomers were synthesized in the following procedure.
Synthetic example 1-1
[0320] [Synthesis Example 1-1] Production of Methacryloyloxyacetyl Chloride
[0321]
[0322] In a 100mL reactor equipped with a condenser, 30g (purity 46%, 95.1mmol) methacryloyloxyacetic acid (there is a description of the production method in the International Publication No. 96 / 41842 pamphlet, etc.), 347mg (4.8 47.6 g (380.5 mmol / 4.0 equivalent) of thionyl chloride was added dropwise to dimethylformamide in mmol / 0.05 equivalent, and stirred at 70° C. for 1 hour. Then, purification was carried out by distillation to obtain 10.0 g of the target methacryloxyacetyl chloride. At this point the purity was 70%, and the yield was 45%.
[0323] [Physical properties of methacryloyloxyacetyl chloride] 1 H NMR (measurement solvent: deuterated chloroform, reference substance: tetramethylsilane): δ=6.22(s, 1H), 5.70(s, 1H), 4.96(s, 2H; CH 2 ), 1.97(s, 3H; CH 3 ).
Synthetic example 1-2
[0324] [Synthesis Example 1-2] Production of 2-bromo-2,2-difluoroethyl trimethylacetate
[0325]
[0326] Into a glass flask equipped with a thermometer, condenser, and dropping funnel were charged 271 g (2.24 mol) of trimethylacetyl chloride, 360 g (2.23 mol) of 2-bromo-2,2-difluoroethanol and 1.5 L of diisopropyl ether and stir. Then, 318 g (3.14 mol) of triethylamine was added dropwise in an ice bath. After completion of the dropwise addition, stirring was continued at room temperature for 1 hour, and the termination of the reaction was confirmed by gas chromatography. 300ml of water was added to the reaction solution to dissolve the entire reaction solution, and then 500ml of 2N hydrochloric acid was added. After separating the organic layer and the aqueous layer, the aqueous layer was extracted with 500 ml of diisopropyl ether. Next, the organic phase was washed with 500 ml of saturated brine, and dried over anhydrous sodium sulfate. Then, the solvent was distilled...
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