HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
Sodium borohydride → (7-(4-Amino-2-fluorophenoxy)thieno[3,2-b]pyridin-2-yl)(pyrrolidin-1-yl)methanone
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | Sodium borohydride | HCID 4311764 | — |
| Edukt | (7-(2-Fluoro-4-nitrophenoxy)thieno[3,2-b]pyridin-2-yl)(pyrrolidin-1-yl)methanone | HCID 59424552 | — |
| Lösungsmittel | MeOH tetrahydrofuran | HCID 21899815 | — |
| Produkt | (7-(4-Amino-2-fluorophenoxy)thieno[3,2-b]pyridin-2-yl)(pyrrolidin-1-yl)methanone | HCID 59424653 | 91,4% |
Reaktionsschritte
To a solution of 22 (3.23 g, 8.33 mmol) and NiCl2.6H2O (3.96 g, 16.66 mmol) in MeOH/THF (100/100 mL) was added NaBH4 (1.24 g, 33.32 mmol). The reaction mixture was stirred for 1 hr, concentrated to dryness and the resultant solid was dissolved in 10% HCl. The aqueous solution was then made basic with concentrated NH4OH solution and extracted with EtOAc. The organic phase was collected, dried over anhydrous sodium sulfate and concentrated under reduced pressure to afford 23 as a black solid (2.72 g, 91% yield). MS (m/z): 358.2 (M+H).
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US08093264B2 |
| Quelldatensatz | uspto-grants-2012_01 |
| ORD ID | ord-c41c3a060d654400a4e9cd6ff5b771ad |
| Quellennotiz | uspto-grants-2012_01 |