To a solution of 3- amino-3-phenylpropionic acid (1.98 g, 12.0 mmol) in THF/H20 (1: 1,40 mL), was added NaOH (1.06 g, 26.4 mmol), and the resulting solution was stirred at rt for 30 min. Di-tert-butyl dicarbonate (2.9 g, 13.2 mmol) was added, and the solution was stirred at rt for 20 h. The solution was concentrated under reduced pressure, diluted with H20 (100 mL), and extracted with Et20 (2 X 150 mL). The aqueous layer was acidified using 1 N HCI, and extracted with EtOAc (2 X 200 mL). The combined organic extracts were washed with brine (200 mL), dried (Na2SO4) and filtered, and the solvent was removed to afford 2.65 g (83percent) of the desired product as a tan solid. MS (electrospray) : mass calculated for C14H19NO4, 265.13 ; m/zfound, 553.3 [2M+Na] +. 1H NMR (400 MHz, CD30D) : 7.37-7. 26 (m, 5H), 5.51 (br s, 1 H), 5.05 (br m, 1 H), 2.98-2. 74 (m, 2H), 1.44 (s, 9H).作者: adg 时间: 2014-6-8 16:39
常规方法就可以吧？
二氯，三乙胺，DMAP作者: ass 时间: 2014-6-8 16:39
来学习学习，这个我不会作者: happydream 时间: 2014-6-8 16:39
我是按照这个条件做的
A 4-L, four-necked, round-bottomed flask, equipped with an efficient stirrer, a dropping funnel,reflux condenser, and thermometer is charged with a solution of 44 g (1.1 mol) of sodium hydroxide in 1.1 L of water. Stirring is initiated and 165.2 g (1 mol) of L-phenylalanine (Note 1) is added at ambient
temperature, and then diluted with 750 mL of tert-butyl alcohol (Note 2). To the well-stirred, clear solution (Note 3) is added dropwise within 1 hr, 223 g (1 mol) of di-tert-butyl dicarbonate (Note 4). A white precipitate appears during addition of the di-tert-butyl dicarbonate. After a short induction period, the temperature rises to about 30–35°C. The reaction is brought to completion by further stirring overnight at room temperature.
反应结束，走液相，发现有新的物质生成，氨基酸已经没有了，但是打H谱，竟然是氨基酸作者: iop 时间: 2014-6-8 16:40
