反应详情

To a suspension of 2-aminomethylphenylacetic acid.HCl (4.0 g, 20 mmol) in H2O (20 ml) was added NaHCO3 (5.0 g, 60 mmol), followed by a solution of Boc-Asp(OcHex)-OSu (7.5 g, 18 mmol) in THF (20 ml). The reaction mixture was stirred at room temperature for 3 hours, filtered, diluted with H2O, acidified with 1N HCl, and extracted with ethyl acetate. The extracts were washed with H2O, brine, dried over anhydrous magnesium sulfate, and evaporated to dryness under reduced pressure. This material was triturated with ether to provide the title compound (7.0 g, 83%) as a white powder. 1H NMR (D6 -DMSO) 12.40 (br s, 1H), 8.30 (br t, 1H), 7.20 (m, 5H), 4.65 (m, 1H), 4.35 (q, 1H), 4.25 (m, 2H), 3.65 (s, 2H), 2.70 (dd, 1H), 2.55 (dd, 1H), 1.70 (m, 4H), 1.40 (s, 9H), 1.35 (m, 6H).

1. filtrationfiltered
2. additiondiluted with H2O
3. extractionextracted with ethyl acetate
4. washThe extracts were washed with H2O, brine
5. dry with materialdried over anhydrous magnesium sulfate
6. customevaporated to dryness under reduced pressure
7. customThis material was triturated with ether