HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
Sodium hydride → Methyl 3-(3,6-Dibromo-9H-carbazol-9-yl)-2-hydroxypropanoate
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | Sodium hydride | HCID 24758 | — |
| Edukt | Methyl oxirane-2-carboxylate | HCID 145751 | — |
| Edukt | 3,6-Dibromocarbazole | HCID 274874 | — |
| Lösungsmittel | Dimethylformamide | HCID 6228 | — |
| Produkt | Methyl 3-(3,6-Dibromo-9H-carbazol-9-yl)-2-hydroxypropanoate | HCID 58097196 | 32% |
Reaktionsbedingungen
| Temperatur | 0 °C |
|---|
Reaktionsschritte
3,6-Dibromocarbazole (0.300 g, 0.923 mmol) was dissolved in DMF (1.2 mL) and cooled to 0° C. NaH (60% dispersion in mineral oil, 0.074 g, 1.846 mmol) was added and the reaction stirred for 1 h at 0° C. Methyl glycidate (0.471 g, 4.615 mmol) was added and the reaction was stirred and warmed to ambient temperature over 3.5 h. Upon completion by TLC the reaction mixture was partitioned between EtOAc and H2O. The aqueous layer was extracted 3× with EtOAc, and the combined organics were washed with saturated aqueous NaCl, dried over Na2SO4, filtered, and concentrated in vacuo. The crude residue was purified by chromatography (SiO2, 0-30% EtOAc/Hexane) to afford the desired product (125 mg, 32%).
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US09446042B2 |
| Quelldatensatz | uspto-grants-2016_09 |
| ORD ID | ord-5388e97b41d842b3a71dd7168ec57a11 |
| Quellennotiz | uspto-grants-2016_09 |