HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
p-Toluenesulfonic acid → 1,3,4,9-Tetrahydro-1,1-diethyl-6-(phenylmethoxy)pyrano[3,4-b]indole
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | p-Toluenesulfonic acid | HCID 6101 | — |
| Edukt | Ethyl ketone | HCID 7288 | — |
| Edukt | 5-Benzyloxy-3-(2-hydroxyethyl)indole | HCID 744849 | — |
| Lösungsmittel | Benzene | HCID 241 | — |
| Produkt | 1,3,4,9-Tetrahydro-1,1-diethyl-6-(phenylmethoxy)pyrano[3,4-b]indole | HCID 19935702 | — |
Reaktionsschritte
A mixture consisting of 5-benzyloxytryptophol (7.0 g, 0.0262 mol), diethyl ketone (10 mL), benzene (400 mL) and p-toluene sulfonic acid is refluxed for 3.5 hours using a Dean-Stark tap to remove the water. The reaction mixture is cooled to room temperature, washed with 5% sodium bicarbonate, water (200 mL), brine (200 mL), dried (MgSO4), filtered and concentrated to give 9.9 g of crude product. The crude product is flash chromatographed on silica gel using 15% ethyl acetate/hexane as an eluent to afford 6.5 g of pure title compound.
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US05420289 |
| Quelldatensatz | uspto-grants-1995_05 |
| ORD ID | ord-a09d1d9c3a1d4cbca6ef532f7dd1bb33 |
| Quellennotiz | uspto-grants-1995_05 |