HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
Phthaloyl chloride → 2-Bromo-4,5-dimethoxyl-(2-phthalimidoethyl)benzene
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | Phthaloyl chloride | HCID 6955 | — |
| Edukt | Diisopropylethylamine | HCID 81531 | — |
| Edukt | 2-Br-4,5-DMPEA | HCID 820370 | — |
| Lösungsmittel | Acetonitrile | HCID 6342 | — |
| Produkt | 2-Bromo-4,5-dimethoxyl-(2-phthalimidoethyl)benzene | HCID 5061742 | — |
Reaktionsschritte
2-Bromo-4,5-dimethoxylbenzeneethanamine (3.5 g 13.2 mmol) was dissolved and stirred in 50 mL dry acetonitrile. 2.14 mL (1.1 equiv) phthaloyl dichloride and 7 mL (3 equiv) Hünig's base were added. The mixture was stirred at room temperature overnight. Acetonitrile was then removed, and the remaining product was taken up in dichloromethane and washed with basic water (pH=11). The aqueous wash was extracted with dichloromethane 3×15 mL. The organic fractions were combined and dried over sodium sulfate. Solvent was removed to give the crude product, which was then purified by column chromatography. Calculated yield: 1.8 g (34%).
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US09302990B2 |
| Quelldatensatz | uspto-grants-2016_04 |
| ORD ID | ord-cc7969ff3c2a4c9bbd52b66808ab44a1 |
| Quellennotiz | uspto-grants-2016_04 |