Method for removing residual metal in organic compounds by using EDTA calcium disodium salts as chelons in liquid phase
A technology for organic compounds and residual metals, used in organic chemistry methods, purification/separation/stabilization of organic compounds, organic chemistry, etc.
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Embodiment 1
[0044] Preparation of 2-amino-6-ethoxy-4-(4-trifluoromethyl-aniline)-pyridine-3-carbaldehyde (Formula 4) for the simultaneous removal of metallic aluminum and nickel.
[0045]
[0046] Formula 3 Formula 4
[0047] 2-Amino-6-ethoxy-4-(4-trifluoromethyl-aniline)-pyridine-3-carbonitrile (176 g) was added to a mixture of pyridine (2600 ml), water (984 ml) and acetic acid (1320 ml) at room temperature. ) in a mixed solvent composed of Wet Raney nickel (type 2800, 120 g) was added under a nitrogen atmosphere. Sodium hypophosphite (168 g) was dissolved in 350 ml of water, and then added in small portions to the reaction mixture to carry out hydrogen transfer reduction reaction.
[0048] After reacting at 80-85°C for 4 hours, it was filtered. The resulting solid was washed twice with pyridine (100 mL each). The combined filtrates were evaporated in vacuo until one-fifth of the volume remained, 2N hydrochloric acid (3800ml) was added and a solid precipitated out immediately, fil...
Embodiment 2
[0053] Preparation of ethyl 5-cyano-2-methyl-benzoate (Formula 6) for removal of residual copper.
[0054]
[0055] Formula 5 Formula 6
[0056] At room temperature, 5-bromo-2-methyl-benzoic acid ethyl ester (24g), copper cyanide (9.2g) and anhydrous N-methylpyrrolidone (80ml) were added into a dry flask filled with nitrogen. Heated to 130°C and reacted at constant temperature for 36 hours. Cool to 20-30°C, add brine (250ml) dropwise, and stir the slurry-like precipitate for 2 hours. After continuing to cool to 5-10°C, the solid was collected and washed twice with water.
[0057] Add the wet crude product containing 1220ppm copper salt into N-methylpyrrolidone (90ml), and heat to 70-80°C to dissolve. EDTA calcium sodium salt solution (0.15N, 50ml) was added to the above hot solution and stirred for 30 minutes, then cooled to 5°C and kept for 2 hours. The solid was collected and washed five times with water until the characteristic blue color of dissolved copper ions in ...
Embodiment 3
[0060] Preparation of acetic acid 2,6,6-trimethyl / 4,6,6-trimethyl-bicyclo[3.1.1]hept-3-ene-2-acetate (Formula 8 and Formula 9), using to remove residual lead.
[0061]
[0062] Formula 7 Formula 8 Formula 9
[0063] (1R)-(+)-α-pinene (25.0g, [α] D 20 +50.9°) and toluene (350ml) were added to the flask, heated to 60-65°C, and palladium acetate (82g) was added in portions to obtain a bright yellow reaction solution. When heated to 65°C and kept at constant temperature for 1 hour, the reaction solution turned yellowish brown, cooled at room temperature and filtered.
[0064] Water (300ml) was added to the filtrate to obtain a brown lead oxide precipitate, which was stirred slowly for 1 hour and then covered with diatomaceous earth for filtration.
[0065] Sampling from the upper layer toluene phase of the filtrate, analysis after concentration, the result shows that the lead content is 2010ppm.
[0066] EDTA calcium sodium salt (12 g) was added to the two-phase filtrate, ...
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