N,N',N",N"'-(Tetrafluorodiborato) bis[μ-(2,3-butanedionedioxiMato)]cobalt(II), Min. 98% synthesis

Yield:-

Reaction Conditions:

in diethyl ether at 20; for 7.75 h;Inert atmosphere;Cooling with ice;Temperature;

Steps:

1; 2; 3; 4; 5; 6; 7; 8; 9; 10; 11; 12; 13; 14; 15; 16; 17; 18; 19; 20; 21; 22; 23; 24; 25; 26; 27; 41; 42; 43; 44; 45; 46; 47; 48; 49 Comparative Example 1 to 8: Synthesis of COBF
Use different reaction times and temperatures. The general procedure is as follows: Cobalt (II) acetate tetrahydrate (2.0 g) and dimethylglyoxime (1.90 g) were added to a 250-ml eggplant type reaction flask under nitrogen atmosphere at room temperature or in an ice water bath.Diethyl ether (150ml), stir and stir for 15 to 30 minutes,The boron trifluoride diethyl ether complex (10 ml) was slowly added dropwise, and the addition was completed in about 30 minutes.Stirring is then continued for 6-9 hours at room temperature or under reflux.The resulting precipitate is separated by filtration, with a small amount of water,Methanol and ether were washed separately and dried.A difluoroborono-bridged ethanedione dioxime cobalt complex is obtained.The crude difluoroborono-bridged ethanedione dioxime cobalt complexis further washed or resuspended in a solvent or ultrasonicated, and then filtered and dried.The purity was then analyzed by ultraviolet-visible absorption spectroscopy. The results obtained are shown in Table 1.

References:

Guangzhou Li Bang Paint Co., Ltd.;Li Bang Industry Paint (Shanghai) Co., Ltd.;Hu Jian;Jiang Longheng CN108530491, 2018, A Location in patent:Paragraph 0079-0080; 0082-0083; 0091; 0104; 0112-0121; 0127