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在最优反应条件[海因2 mmol,n(3-戊酮)∶n(海因)=1.5,乙醇胺为碱,p H 4,于55℃反应6 h]下制得5-(1-乙基亚丙基)海因(4);4用5%Pd/C催化加氢制得5-(3-戊基)海因(5);5先在碱性条件下水解,再通过叔丁氧羰基保护氨基合成了(±)-N-叔丁氧羰基-3-乙基-戊氨酸,总收率43%,其结构经~1H NMR,~(13)C NMR和HR-ESI-MS确证。
The yield of 5- (1- (4-hydroxyethyl) -1-methyl-2-pyrimidin-4-one) was optimized under the optimal reaction conditions [ Ethylpropyl) hydantoin (4); 4 Hydrogenation of 5- (3-pentyl) hydantoin with 5% Pd / C; 5 Hydrolysis under basic conditions followed by tert- (±) -Nt-Butyloxycarbonyl-3-ethyl-glutanoic acid was synthesized in the total yield of 43%. The structure was confirmed by ~ 1H NMR, ~ 13CNMR and HR-ESI -MS confirmation.