N,N'-BIS(SALICYLIDENE)-1,4-BUTANEDIAMINE synthesis

Yield:3955-57-5 96.8%

Reaction Conditions:

in N,N-dimethyl-formamide at 20; for 6 h;

Steps:

6.I

Example 6; Three-stage synthesis of the compound P-C₄-Bz; Three-stage synthesis of P-C₄-Bz: Stage (I) Synthesis of the intermediate product C₄-HB; Stage (II) Synthesis of the intermediate product P-C₄-HB; Stage (III) Synthesis of the monomer P-C₄-Bz. The reaction is as follows: Stage (I) Synthesis of the intermediate product C₄-HB. 2-HB 13.8515 g (56.75×2 mmol) and 1,4-butanediamine 5 g (56.75 mmol) are dissolved in 50 ml DMF within a three-neck flask, and stirred under nitrogen until slightly exothermic. Under room temperature, keep stirring for 6 hours for maximum precipitates. The mixture is poured into de-ionized water for precipitates. After filtration, vacuum evaporation and vacuum oven at 70° C., 21.6273 g yellow powder 4-HB is obtained with a yield rate of 96.8%. Melting point 91° C. The results are shown in FIG. 4A. FIG. 4A is 1H-NMR spectrum of the intermediate product C₄-HB. The structure of the synthesized C₄-HB can be verified by the figure.

References:

US2009/171120,2009,A1 Location in patent:Page/Page column 18