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2Â¥2010-06-01 14:43:22
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ÎÄÏ×¶¼×öµ½¹«½ï¼¶ÁË£¬²»¿ÉÄÜÊÇ·´Ó¦±¾ÉíµÄÎÊÌâÎÄÏ×ÃèÊöÊÇ 4-amino-3,6dichloropyridine-2-carboxylic acid (batch cell) The cell was a 180 mL beaker (2 in. (5.1 cm) diameter x 4.5 in. (11.4 cm) tall). The silver mesh cathode consisted of a 1 in. (2.5 cm) x 4 in. (10.2 cm) strip placed around the inside wall of the beaker approximately 0.5 in. (1.3 cm) off the bottom and had a 0.5 in. (1.3 cm) wide strip extending out the top of the beaker to which the power supply was attached. The anode was a 0.75 in. (1.9 cm) diameter x 6 in. (15.2 cm) long graphite rod that was supported by a rubber stopper in the middle of the beaker and extended to about 0.5 in. (1.3 cm) off the bottom. The working potential of the cathode was controlled relative to an Ag/AgCl (3.0 M Cl-) reference electrode positioned between the silver mesh and the wall of the beaker. The silver mesh cathode was activated by anodization at +0.7 volt (v) in a 2% sodium hydroxide and 1% sodium chloride solution in water followed by reverse polarization. After activation, the solution was replaced with a solution of 81 mL of water, 5.1 g (0.0213 moles) of 4-amino-3,5,6-trichloropicolinic acid, and 2.8 g (0.0426 moles) of 85% KOH. After sparging with a slow stream of nitrogen, the electrolysis was carried out at a working potential of -1.3 to-1.35 volts for 2 hours at ambient temperature. The current started at 0.83 amps and gradually decreased to 0.25 amps after the two hours. A total of 5000 coulombs were passed through the solution (theory for reduction of one chlorine off the pyridine ring is 2050 coulombs). Analysis of the crude product solution by gradient elution HPLC showed the disappearance of the starting material and the appearance of a single peak later identified as 4amino-3,6-dichloropicolinic acid ´ó¼Ò¿´¿´ÎÒ·´Ó¦ÓÐÎÊÌâÂ𣿠ÒÔǰû×ö¹ýµç»¯Ñ§£¬º¹ |
3Â¥2010-06-01 15:07:36
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5Â¥2010-06-01 20:08:50
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6Â¥2010-06-02 12:48:16
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