2018-61-3

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Material Safety Data Sheet(MSDS)

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• Preparation

  The catalytic hydrogenation activity of N-acetyl-(S)-phenyl methyl esters was measured under controlled pressure and temperature conditions in a conventional low-pressure hydrogenator (Parr Inst. Co., Mod. 3911). Hydrogenation was carried out in methanol as a solvent with 20 mL of 0.80 M substrate solution and 0.034 g of cis-Δ-(R)-(S)-2.5H₂O (Scheme 1), yielding [subs]/[cat] = 0.016/0.000029 = 547 under all conditions, with an initial hydrogen pressure of 6.8 atm and a temperature of 50–70°C. Methanol (99%, Scharlau) and hydrogen (99.999% SEO) were added to the reaction mixture. Methyl acetoacetate and 1-hexene were added. The mixture was distilled under reduced pressure and at low temperature. Dimethyl itaconic acid and methyl 2-acetamidoacrylate, supplied by Aldrich, were added. The reaction mixture was refluxed with a boron trifluoride-methanol complex (Merck). The hydrogenation product was purified by a Konik-3000 gas chromatograph equipped with a Supelco (BETA DEX 120) β-cyclodextrin chiral column to give the product N-acetyl-L-phenylalanine.;

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