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N-(O-(3-maleinimidobenzoyl)-2-hydroxyethyl)-N,N'-bis-tertiarybutyloxycarbonyl-1,2-diaminoethane To a solution of 8 g (26.3 mmol) <strong>[200283-08-5]N-(2-hydroxyethyl)-N,N'-bis-tertiarybutyloxycarbonyl-1,2-diaminoethane</strong> in 50 ml of tetrahydrofuran and 4 ml (28.9 mmol, 1.1 eq) of triethylamine, 6.82 g (29 mmol, 1.1 eq) of maleinimidobenzoic acid chloride, dissolved in 100 ml of tetrahydrofuran, are added drop-wise at room temperature while stirring within 1 h. After stirring for a further 8 h at room temperature, according to DC, the reaction is completed. The triethylammonium chloride formed in the reaction is filtered off. After removal of the tetrahydrofuran and the excess triethylamine under a vacuum, the oil formed is purified using column chromatography (silica gel: ethyl acetate/hexane (1:1), Rf-value (ethyl acetate/hexane 1:1)=0.2, yield: 9.6 g (19.1 mmol) of the product in the forM a yellow oil, corresponding to 72.6% of the theoretically possible yield.
EXAMPLE 25 N-(1-cyclohexyl-2-pyrrolidinyl-methyl)-2-methoxy-4-amino-5-ethylsulphonyl-benzamide Using a 1 liter flask fitted with an agitator, a thermometer and a dropping funnel, 98 g of 2-methoxy-4-amino-5-ethylsulphonyl-benzoic acid (0.378 mole) is dissolved in 392 ml of acetone, then 38 g of triethyl amine (0.378 mole) is added. The triethyl amine salt of the organic acid crystallises immediately. The suspension is cooled to 0° C. then 41 g of ethyl chlorofomate (0.378 mole) is added drop by drop between 0° and 5° C. The salt is dissolved gradually and the triethylamine hydrochloride is precipitated in fine white crystals.
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