HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
1-Iodohexane → 2-[4-[N-acetyl-N-(3-phthalimidopropyl)amino]-3-fluorophenyl]-6,8-difluoro-5-hexylamino-4H-1-benzopyran-4-one
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | 1-Iodohexane | HCID 12527 | — |
| Edukt | Sodium hydride | HCID 24758 | — |
| Edukt | Ammonium Chloride | HCID 25517 | — |
| Edukt | 2-[4-[N-Acetyl-N-(3-phthalimidopropyl)amino]-3-fluorophenyl]-5-amino-6,8-difluoro-4H-1-benzopyran-4-one | HCID 15346994 | — |
| Lösungsmittel | Dimethylformamide | HCID 6228 | — |
| Produkt | 2-[4-[N-acetyl-N-(3-phthalimidopropyl)amino]-3-fluorophenyl]-6,8-difluoro-5-hexylamino-4H-1-benzopyran-4-one | HCID 19434853 | 35% |
Reaktionsschritte
450 mg of Compound 28 was dissolved in 15 ml of dimethylformamide, 0.62 ml of 1-iodohexane and 34 mg of sodium hydride (60% oil dispersion) were added under ice-cooling and the mixture was stirred at room temperature for 2 hours. An aqueous solution of ammonium chloride was added, the reaction solution was concentrated under reduced pressure and the residue was extracted once with chloroform. The chloroform layer was washed with an aqueous saturated solution of sodium chloride, dried over anhydrous sodium sulfate and concentrated under reduced pressure. The residue was subjected to silica gel column chromatography (n-hexane:ethyl acetate=1:1-1:3) to give 184 mg (35%) of Compound 31.
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US05539112 |
| Quelldatensatz | uspto-grants-1996_07 |
| ORD ID | ord-11a3c305d37d4c018bdc7b9eb71573db |
| Quellennotiz | uspto-grants-1996_07 |