反应详情

To a solution of the product of step c above (110 mg, 0.22 mmol) in 1:1 THF/methanol (2 ml) was added the solution of lithium hydroxide monohydrate (30 mg, 0.66 mmol) in water (1 ml). The solution was stirred at room temperature for 16 h, concentrated under reduced pressure, diluted with water (1 ml) and acidified (pH=2.0, 1M HCl). The precipitate was collected by filtration, washed with water and dried to afford the title compound as a white solid (92 mg, 89%). 1H NMR (300 MHz, d6-DMSO) 13.00 (2H, br s), 10.23 (1H, s), 8.64 (2H, s), 8.15 (1H, s), 7.92 (1H, s), 7.32 (3H, m), 7.14 (2H, m), 5.28 (2H, s), 2.83 (2H, d), 1.51 (5H, m), 1.37 (4H, m), 1.14 (4H, m). The acid was converted to the di(N-methyl-D-glucamine) salt and lyophilised from water/dioxan. Found: C, 54.47; H, 7.63; N, 7.59%; C41H63N5O15.2.2 H2O requires: C, 54.35; H, 7.50; N, 7.73%.

1. concentrationconcentrated under reduced pressure
2. additiondiluted with water (1 ml)
3. filtrationThe precipitate was collected by filtration
4. washwashed with water
5. customdried