化学合成
化学合成
合成路线 1(1. 合成:21461-84-7)
产率:91.6%
合成条件:With hydrogenchloride; sodium nitrite In water at -5 - 20℃; Inert atmosphere
实验步骤:向L-谷氨酸(10.07g,0.068mol,JK CHEMICA)在20ml锥形溶液中的溶液中。 在-5℃下,向HCl和40mL H₂O中缓慢加入NaNO₂(7.0g,0.102mol,汕头西龙化学工厂)在H₂O(20mL)中的溶液。 将混合物在室温下继续搅拌12小时。 将反应混合物在低于50℃下真空蒸发,得到黄色油状物,将其溶解在EtOAc中。 过滤形成的固体并用EtOAc洗涤。 合并滤液和洗涤溶液,用Na₂SO₄干燥。 将溶剂真空浓缩,得到(S)-四氢-5-氧代呋喃-2-羧酸,为浅黄色油状物(8.1g,91.6%),MS(ESI,阳离子)m/z:130.9(M + 1); ¹H NMR(400MHz,CDCl₃):δ2.27-2.41(m,1H),2.44-2.65(m,3H),5.09(m,1H),9.12-9.55(m,1H)。
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