HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
Formaldehyde → 1-(2,3-Dihydro-1,4-benzodioxin-6-yl)-3-(dimethylamino)propan-1-one
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | Formaldehyde | HCID 712 | — |
| Edukt | Dimethylamine, hydrochloride | HCID 10473 | — |
| Edukt | 1,4-Benzodioxan-6-yl methyl ketone | HCID 76143 | — |
| Katalysator | Hydrochloric Acid | HCID 313 | — |
| Lösungsmittel | Ethanol | HCID 702 | — |
| Produkt | 1-(2,3-Dihydro-1,4-benzodioxin-6-yl)-3-(dimethylamino)propan-1-one | HCID 2825018 | 82% |
Reaktionsschritte
A solution of 1-(2,3-dihydrobenzo[b][1,4]dioxin-6-yl)ethanone (XV) (11 mmol), dimethylamine hydrochloride (14 mmol), paraformaldehyde (16 mmol) and 12 N HCl (2 drops) in ethanol (5 mL) was refluxed overnight. The solution was cooled to room temperature and the ethanol was evaporated under vacuum. The residue was treated with ethyl acetate, heated slightly and sonicated to disperse into fine particles. The solids were filtered and dried at room temperature to produce 1-(2,3-dihydrobenzo[b][1,4]dioxin-6-yl)-3-(dimethylamino)propan-1-one (XVI) as a white solid, (82% yield), 1H NMR (CDCl3, 400 MHz): δ ppm 2.77 (s, 6H), 3.41 (m, 2H), 3.56 (m, 2H), 4.25 (m, 4H), 6.85 (m, 1H), 7.45 (m, 2H).
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US08609717B2 |
| Quelldatensatz | uspto-grants-2013_12 |
| ORD ID | ord-4349373024974d779f9d75d81ecb11a8 |
| Quellennotiz | uspto-grants-2013_12 |