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ChemicalBook CAS DataBase List (+/-)-1,2-DIPHENYLETHYLENEDIAMINE

(+/-)-1,2-DIPHENYLETHYLENEDIAMINE synthesis

10synthesis methods
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Yield: 98%

Reaction Conditions:

with pyrographite;hydrazine hydrate in methanol at 58 - 62;Inert atmosphere;Solvent;Reagent/catalyst;Temperature;

Steps:

1
1,2-diphenylethanedione dioxime (48 g, 0.20 mol) and 260 ml of methanol were placed in a 500 ml four-necked flask equipped with a condenser, and the whole was dissolved by stirring. Then, 2 g of activated carbon (120 mesh) 0.5 g Raney nickel, heated to 60 ° C,80% hydrazine hydrate (28.75g,0.46mol) was slowly added dropwise, keeping the reaction temperature at 58°C -62°C The reaction process was controlled by nitrogen gas, and the dropping speed was controlled to be too fast for nitrogen gas release. Chromatography tracks the progress of the reaction. When the starting 1,2-diphenylethanedione dioxime disappears, the reaction is terminated, the mixture is cooled, Raney nickel and activated carbon are filtered, covered with a small amount of water and the filtrate was distilled to recover the methanol. The residue was dissolved in 200 ml of petroleum ether, and the product was dissolved for 24 hours. The product was filtered to obtain (±) 1,1-diphenylethylenediamine in a yield of 98%. Chemical purity 99. 57% •

References:

LianYunGang Chiral Chemical(China)CO.,LTD;Chen, Guosheng CN105218380, 2016, A Location in patent:Paragraph 0031-0034

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