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With hydrogenchloride; In 1,4-dioxane; at 20℃; for 2.0h;
(Comparative Example 5) The compound in Comparative Example 5 was synthesized according to the method described in the Patent document 2: ethyl(2S,4S)-1-tert-butoxycarbonyl-4-(phenylsulfanyl)pyrrolidine-2-carboxylate, prepared from ethyl(2S,4R)-1-tert-butoxycarbonyl-4-(4-toluenesulphonyloxy)-pyrrolidine-2-carboxylate and thiophenol, was hydrolyzed with sodium hydroxide and then the product was treated with 4 M hydrochloric acid in dioxane at room temperature for 2 hours to afford the deprotected compound.
With water; sodium hydrogencarbonate; sodium carbonate; In acetone; at 15 - 20℃;pH 8 - 10;Large scale reaction;
General procedure: The (S)-amino acid (10.0 g) was dissolved in H2O (300 ml) and Na2CO3 (2.0 equiv) and NaHCO3 (1.0 equiv) were added at rt, with stirring, to give a clear solution. Acetone (4.0 vol, with respect to the amino acid) was added and the slightly turbid solution was cooled in an ice water bath to 15-20 C. Cbz-Cl (1.25 equiv) was added slowly, with stirring, and the reaction mixture allowed to warm to rt. After stirring for an additional 3 h at rt the mixture was extracted with Et2O (50 ml). To the aqueous phase was slowly added aqueous HCl to give a pH of 2. The resulting oil was extracted into EtOAc (150 ml) and this was washed with H2O (100 ml) and then concentrated in vacuo to give the N-Cbz amino acid as a white solid, see Table 1.
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