HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
Hydrochloric Acid → 7-(3-Difluoromethylphenyl)-isoquinoline-5-sulfonic acid (2-amino-ethyl)-amide
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | Hydrochloric Acid | HCID 313 | — |
| Edukt | {2-[7-(3-Difluoromethylpheny)-isoquinoline-5-sulfonylamino]-ethyl}-carbamic acid tert-butyl ester | HCID 69327854 | — |
| Lösungsmittel | Ethyl Acetate | HCID 8857 | — |
| Lösungsmittel | 1,4-Dioxane | HCID 31275 | — |
| Produkt | 7-(3-Difluoromethylphenyl)-isoquinoline-5-sulfonic acid (2-amino-ethyl)-amide | HCID 11280346 | 95% |
Reaktionsschritte
Suspend {2-[7-(3-difluoromethylpheny)-isoquinoline-5-sulfonylamino]-ethyl}-carbamic acid tert-butyl ester in ethyl acetate (11 mL), and add an excess of 4 M HCl in 1,4-dioxane. Stir overnight, filter the precipitate, wash with dichloromethane, and dry under vacuum to give the desired compound as a white solid (0.092 g, 95% yield): 1H NMR (CD3OD): δ9.92 (s, 1H), 9.10 (d, J=7.0 Hz, 1H), 9.04 (m, 2H), 8.80 (d, J=7.0 Hz, 1H), 8.09 (m, 2H), 7.74 (m, 2H), 6.94 (t, J=52.1 Hz, 1H), 3.25 (m, 2H), 3.15 (m, 2H). Load the product onto ion exchange resin and elute with 1N NH3 in methanol and concentrate to dryness to give the free base. (Used in example 97).
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US07449477B2 |
| Quelldatensatz | uspto-grants-2008_11 |
| ORD ID | ord-475d33fdef1f433eaf509d5d1b9b4628 |
| Quellennotiz | uspto-grants-2008_11 |