HuagongsheHuagongshe Chemistry Print Report · For research reference only
Methanesulfonic Acid → 5-(2-amino-ethoxy)-6-fluoro-3-(1H-pyrrol-2-yl)-1H-benzo[cd]indol-2-one methanesulfonic acid salt
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Methanesulfonic Acid | HCID 6395 | — |
| Reactant | 5-(2-Amino-ethoxy)-6-fluoro-3-(1H-pyrrol-2-yl)-1H-benzo[cd]indol-2-one | HCID 9836341 | — |
| Solvent | 1,4-Dioxane | HCID 31275 | — |
| Product | 5-(2-amino-ethoxy)-6-fluoro-3-(1H-pyrrol-2-yl)-1H-benzo[cd]indol-2-one methanesulfonic acid salt | HCID 18624487 | — |
Reaction Steps
5-(2-Amino-ethoxy)-6-fluoro-3-(1H-pyrrol-2-yl)-1H-benzo[cd]indol-2-one (from Example 19 above) (62.3 mg, 0.20 mmol) was dissolved in hot 1,4-dioxane (2.5 mL) and the solution was filtered through a glass filter. To the clear filtrate was added dropwise a solution of methanesulfonic acid (Aldrich, 16.0 mg, 0.16 mmol) in 1,4-dioxane (0.2 mL) at room temperature and the mixture was stirred for 10 minutes. The precipitate formed was collected and washed with 1,4-dioxane, ether and dried in vacuo to afford 5-(2-amino-ethoxy)-6-fluoro-3-(1H-pyrrol-2-yl)-1H-benzo[cd]indol-2-one methanesulfonic acid salt as a yellow solid. (Yield 52.5 mg, 64.5%).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06504034B2 |
| Source dataset | uspto-grants-2003_01 |
| ORD ID | ord-da929dfc346b475189d7e775e1e0c6d7 |
| Source note | uspto-grants-2003_01 |