反応 #7308

反応方程式

cis-(1-benzyl-4-methyl-piperidin-3-yl)-methyl-amine

HCl

→

Cis-(1-Benzyl-4-methyl-piperidin-3-yl)-methyl-amine hydrochloride salt

収率 37.5%

溶媒

ethanol

反応条件

後処理

1. 1
   その他at 0° C
2. 2
   その他stayed below 10° C
3. 3
   濃縮Next 3 mis ethanol (2 volumes) were concentrated from the reaction
4. 4
   workup.ADDITIONTo the reaction was charged 7.5 mls ethyl acetate (5 volumes)
5. 5
   その他6 mls ethyl acetate (4 volumes) were removed in vacuo
6. 6
   workup.ADDITION7.5 mls ethyl acetate (5 volumes) were again charged
7. 7
   濃縮the concentration
8. 8
   workup.ADDITIONNext, 4.5 mls acetone (3 volumes) were added
9. 9
   その他to afford white solids

実験手順

The final salt formation was performed by charging 1.5 grams cis-(1-benzyl-4-methyl-piperidin-3-yl)-methyl-amine (1 equiv., 5.15 mmol) and 4.5 ml ethanol (3 volumes) to a reactor at 0° C. To the 0° C. pot, was charged 0.93 ml 36% HCl (0.625 volumes) so that the temperature stayed below 10° C. Next 3 mis ethanol (2 volumes) were concentrated from the reaction. To the reaction was charged 7.5 mls ethyl acetate (5 volumes), the reaction was stirred for 5 minutes and then 6 mls ethyl acetate (4 volumes) were removed in vacuo. 7.5 mls ethyl acetate (5 volumes) were again charged and the concentration was again performed. Next, 4.5 mls acetone (3 volumes) were added and the reaction was slowly cooled to 0° C. in order to afford white solids. (37.5% yield). 1H NMR: δ7.78-7.76 (2 H, d, J=8.0 Hz), 7.29-7.18 (5 H, m, aromatic protons), 5.55 (1 H, s), 3.45-3.41 (1 H, d, J=13.2 Hz), 3.39-3.36 (1 H, d, J=13.2 Hz), 2.79 (1 H, brs), 2.63 (1 H, brs), 2.45 (3 H, s), 2.30 (2 H, s), 2.25-2.05 (1H, m), 1.76 (1 H, brs), 1.40-1.39 (2 H, m), 0.875-0.845 (3 H, d, J=12).

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