2,6-di-tert-butyl-4-methyl-phenol; sodium salt of phosphorous acid; 1-methyl-pyrrolidin-2-one;
reactants are commercially availlable.
saltigo gmbh, us2012/283468, a1, (2012) 2. preparation of methyl 2-fluoroacrylatean amount of di-tert-butylhydroxytoluene (bht) of 4 g (0.02 mol), 500 g of n-methylpyrrolidine (nmp) and 360 g (2.2 mol) of tribasic sodium phosphate are intro duced into a sulfonation pan and the mixture is heated to 150°c. an amount of di-tert-butylhydroxyt oluene (bht) of 51 mg (2.2*10-4 mol) is introduced into the distillation receiver of the vertical re covery bend. a vacuum of 300 mbar is applied and the metered addition of a total of 287 g (98percent, 2.0 mol) of methyl 3-chloro-2-fluoropropionate is begun. the metered addition is continued in the degree in which the methyl 2-fluoroacrylate is distilled over. when no more distillate stream passes over, the vacuum is lowered to 150 mbar. when no more product passes over even here, the pressure i s raised by addition of nitrogen. the distillation bottoms are cooled and discharged via the bottom valve. the product is obtained after distillation as a colorless liquid (205 g, 95percent, 1.87 mol, 93.5percent yield).
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