[CH3:1][O:2][C:3]1[CH:4]=[C:5]([C@H:9]([CH2:16][CH3:17])[C@@H:10]([CH3:15])[CH2:11][N:12]([CH3:14])[CH3:13])[CH:6]=[CH:7][CH:8]=1.COC1C=C([C@@H](CC)[C@@H](C)CN(C)C)C=CC=1.B(O)(O)[C@H]1N(C([C@@H](N)C(C)C)=O)CCC1.CS(O)(=O)=O.[ClH:55]>CC(C)=O>[ClH:55].[CH3:1][O:2][C:3]1[CH:4]=[C:5]([C@H:9]([CH2:16][CH3:17])[C@@H:10]([CH3:15])[CH2:11][N:12]([CH3:14])[CH3:13])[CH:6]=[CH:7][CH:8]=1A mixture of (2R,3R)-3-(3-methoxyphenyl)-N,N,2-trimethylpentan-1-amine and (2R,3S)-3-(3-methoxyphenyl)-N,N,2-trimethylpentan-1-amine (10 kg, 42.56 mol, ratio 5.5:1) was dissolved in acetone (50 L) in a 100 L double jacket vessel equipped with an electrical impeller stirrer, a gas transition line, Pt100 temperature measuring equipment and an oil based cooling/heating system. Hydrogen chloride (1.55 kg, 42.51 mol) was transferred within 15 minutes at a temperature of 5° C. to 25° C. through the reaction mixture. The reaction mixture was cooled to 0° C. to 5° C. and centrifuged after 2 hours of stirring. The humid solid was put into a stirring vessel, acetone (30 L) was added and the reaction mixture was heated to reflux for 15 minutes. After cooling to 15° C. to 20° C. the product was centrifuged and stored at 40° C. to 50° C. and 150 mbar for 14 hours in a drying oven. (2R,3R)-3-(3-Methoxyphenyl)-N,N,2-trimethylpentan-1-amine hydrochloride (7.17 kg, 63%) was obtained as a colorless solid with a diastereomeric excess of 100%.
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