反应详情

5-(2-Amino-ethylamino)-6-fluoro-3-(1H-pyrrol-2-yl)-1H-benzo[cd]indol-2-one (from Example 9 above) (1.38 g, 4.4 mmol) was dissolved in hot 1,4-dioxane (100 mL) and the solution was filtered through a glass filter. To the clear filtrate was added dropwise a solution of methanesulfonic acid (Aldrich, 380 mg, 3.95 mmol) in 1,4-dioxane (5 mL) at room temperature and the mixture was then allowed to stir for 10 minutes. The precipitate was collected and washed with 1,4-dioxane, ether and dried in vacuo to give the crude product (1.52 g) which was re-crystallized from DMF/1,4-dioxane (14 mL/50 mL) to afford 5-(2-amino-ethylamino)-6-fluoro-3-(1H-pyrrol-2-yl)-1H-benzo[cd]indol-2-one methanesulfonic acid salt as a dark green solid. (Yield 1.0 g, 55.9%).

1. filtrationthe solution was filtered through a glass
2. filtrationfilter
3. customThe precipitate was collected
4. washwashed with 1,4-dioxane, ether
5. customdried in vacuo
6. customto give the crude product (1.52 g) which
7. customwas re-crystallized from DMF/1,4-dioxane (14 mL/50 mL)