反应详情

Fmoc-Lys(Mtr) 1 (5.25 g, 8.19 mmol) in 1:1 methylene chloride/acetonitrile (80 mL) at rt was treated with diethylamine (80 mL). After 1.5 h the solvents were evaporated. The residue was flushed with acetonitrile (2×50 mL) at 60° C., and then triturated with ether (80 mL). The resulting solid was collected by filtration, washed with ether, and then dissolved as far as possible in 1:1 methylene chloride/methanol. Some solid byproduct was removed by filtration and the filtrate was concentrated invacuo. The resulting light tan solid was dried in vacuo for 4 h (3.2221 g, 94%). 1H-NMR (DMSO-d6) δ 1.34, 1.57 and 1.72 (m, 6H), 2.05 (m, 2H), 3.38 (m, 1H), 3.68 (s, 3H), 3.71 (d, 2H), 7.03-7.40 (m, 12H). MS (FAB) 419.2 (MH)+, 441.4 (M+Na)+, 457.4 (M+K)+. MS (FAB) 419.2 (MH)+, 441.4 (M+Na)+, 457.4 (M+K)+.

1. customAfter 1.5 h the solvents were evaporated
2. customThe residue was flushed with acetonitrile (2×50 mL) at 60° C.
3. customtriturated with ether (80 mL)
4. filtrationThe resulting solid was collected by filtration
5. washwashed with ether
6. dissolutiondissolved as far as possible in 1:1 methylene chloride/methanol
7. customSome solid byproduct was removed by filtration
8. concentrationthe filtrate was concentrated invacuo
9. customThe resulting light tan solid was dried in vacuo for 4 h (3.2221 g, 94%)