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ChemicalBook CAS DataBase List (S)-(-)-N,N-DIMETHYL-1-FERROCENYLETHYLAMINE

(S)-(-)-N,N-DIMETHYL-1-FERROCENYLETHYLAMINE synthesis

3synthesis methods
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Yield:31886-57-4 89%

Reaction Conditions:

Stage #1: 1-ferrocenylethanolwith acetic anhydride;triethylamine in dichloromethane at 20; for 3 h;Large scale;
Stage #2: dimethyl amine in dichloromethane;water; for 5 h;Large scale;Temperature;Solvent;

Steps:

5.3

(3) (S)-1-ferrocenylethanol 2 (1.03 kg, 4.47 mol) prepared above, dichloromethane (3.0 L),Triethylamine (902.9 g, 8.94 mol) was placed in the reaction vessel in turn, acetic anhydride (683.4 g, 6.70 mol) was added dropwise at room temperature, and the reaction was stirred for 3 h;Then slowly add 4.31kg of 33% dimethylamine aqueous solution, continue stirring for 5h; static layering, concentration and concentration to recover dichlorohexane.The residue was distilled under reduced pressure to collect a fraction of 110 ° C (0.07 kPa) to obtain (S)-N,N-Dimethyl-1-ferrocenylethylamine 3 (1.02 kg).Dark red oily liquid, yield: 89%; HPLC purity: 98%; ee: 96%.

References:

CN108409802,2018,A Location in patent:Paragraph 0050; 0053

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