HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
Sodium Thiosulfate → 2-[4-(1,4-Dioxa-7-aza-spiro[4.4]non-7-yl)-3-fluorophenyl]-6-methoxy-2H-isoquinolin-1-one
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | Sodium Thiosulfate | HCID 24477 | — |
| Edukt | Triacetoxyperiodinane | HCID 159087 | — |
| Edukt | N-[4-(1,4-dioxa-7-aza-spiro[4.4]non-7-yl)-3-fluorophenyl]-2-(2-hydroxyethyl)-4-methoxy-benzamide | HCID 68989883 | — |
| Lösungsmittel | Dichloromethane | HCID 6344 | — |
| Produkt | 2-[4-(1,4-Dioxa-7-aza-spiro[4.4]non-7-yl)-3-fluorophenyl]-6-methoxy-2H-isoquinolin-1-one | HCID 68990227 | — |
Reaktionsschritte
Dess-Martin periodinane (7 g) was added to a solution of N-[4-(1,4-dioxa-7-aza-spiro[4.4]non-7-yl)-3-fluorophenyl]-2-(2-hydroxyethyl)-4-methoxy-benzamide (4.6 g) in methylene chloride (279 mL). The reaction mixture was stirred for 2 h at room temperature, then further Dess-Martin periodinane (1.4 g) was added, stirring for a further 4 h at room temperature. Then 5% Na2S2O3 solution was added to the reaction solution and the organic phase was then washed with water. The methylene chloride phase was dried over sodium sulfate and the solvent was removed in vacuum. The raw product was purified by preparative HPLC. In this way the product was obtained with molecular weight 396.15 (C22H21FN2O4); MS (ESI): 397 (M+H+).
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US08822495B2 |
| Quelldatensatz | uspto-grants-2014_09 |
| ORD ID | ord-aa94c331bfbc44178c5186fc0abceb12 |
| Quellennotiz | uspto-grants-2014_09 |