反应 #2958944
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openreactiondata ↗doi:10.6084/m9.figshare.5104873.v1; patent:US09353114B2
反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.
实验步骤: (c)Preparation of (R)—N-piperidin-3-ylacetamide Dibenzyol tartarate salt: In a RBF charged 500 ml of Methanol, 50 gm of N-piperidin-3-ylacetamide & 138 gm of L (+)-Dibenzoyl tartaric acid. The reaction was maintained for about 90 mins at room temperature and then heated to reflux. The reaction mass was maintained for about an hour at reflux and then cooled and maintained at room temperature for about 12.0 hours. Then, the product was filtered and washed with 100 ml methanol. Again charged the obtained wet cake in 800 ml methanol, heated to reflux and maintained reaction mass for 1.0 hr to get a clear solution. Cooled the reaction mass to room temperature and maintained for 12.0 hrs. The product was filtered and washed with 100 ml methanol. The product was dried at about 45-50° C. under vacuum. Unwanted S-isomer NMT 1.5% Dry Wt-20. Gm. heated to reflux The reaction mass was maintained for about an hour at reflux cooled maintained at room temperature for about 12.0 hours Then, the product was filtered washed with 100 ml methanol Again charged the obtained wet cake in 800 ml methanol heated to reflux maintained reaction mass for 1.0 hr to get a clear solution Cooled the reaction mass to room temperature maintained for 12.0 hrs The product was filtered washed with 100 ml methanol The product was dried at about 45-50° C. under vacuum Unwanted S-isomer NMT 1.5% Dry Wt-20
来源 ID: ord-6e45b9d26e444187a3c8d80cfad13703