反应详情

A stirred solution of Fmoc-Lys(Mtr)-OSu 3 (ca 8.672 mmol) and Lys(Mtr) 2 (3.6294 g, 1 equiv) in DMF (70 mL) at rt was treated with DIEA (4.5 mL, 3 equiv). After 4 h the mixture was diluted with ethyl acetate (250 mL). The solution was washed with pH 4 buffer (0.05M biphthalate) (2×), water and brine, dried over sodium sulfate and evaporated the residue was flushed with methylene chloride (400 mL) to give a pale-yellow foam which was carried on without further purification. 1H-NMR (CDCl3/CD3OD) δ 1.10-1.85 (m, 12H), 2.22 (m, 4H), 3.70 (m, 6H), 4.21 (m, 5H), 6.76 (m, 4H), 7.00-7.75 (m, 32H). MS (ESI) 1041. 6 (MH)+.

1. washThe solution was washed with pH 4 buffer (0.05M biphthalate) (2×), water and brine
2. dry with materialdried over sodium sulfate
3. customevaporated the residue
4. customwas flushed with methylene chloride (400 mL)
5. customto give a pale-yellow foam which
6. customwas carried on without further purification