HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
3-Methyl-2-butanone → HCID 66726288, Verbindung
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | 3-Methyl-2-butanone | HCID 11251 | — |
| Edukt | Sodium Hydroxide | HCID 14798 | — |
| Edukt | 3,4-dihydro-2H-1,5-benzodioxepine-7-carbaldehyde | HCID 2776388 | — |
| Lösungsmittel | Methanol | HCID 887 | — |
| Produkt | HCID 66726288 | HCID 66726288 | — |
Reaktionsschritte
The MeOH (5 mL) solution of 3,4-dihydro-2H-1,5-benzodioxepine-7-carbaldehyde (445 mg) and 3-methyl-2-butanone (195 mg) was treated with aq. sodium hydroxide (1N, 1 ml) and the mixture was stirred for 24 hours. The reaction was partitioned between 10 ml water and 40 ml ethyl acetate. The organic layer was then sequentially washed with aq. hydrochloric acid (1N, 20 ml), water (20 ml), and Brine (20 ml) and then concentrated under reduced pressure. The residue was purified with flash chromatography on silica (33% ethyl acetate in hexane) to give the desired product as a white crystal.
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US08722896B2 |
| Quelldatensatz | uspto-grants-2014_05 |
| ORD ID | ord-92691c7ded8f4b29ac0610f63ab42051 |
| Quellennotiz | uspto-grants-2014_05 |