HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
Hydrochloric Acid → 2,3-Dihydroxy-4-methoxybenzaldehyde
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | Hydrochloric Acid | HCID 313 | — |
| Edukt | Boron Trichloride | HCID 25135 | — |
| Edukt | 2,3,4-Trimethoxybenzaldehyde | HCID 75006 | — |
| Edukt | Sodium Bicarbonate | HCID 516892 | — |
| Lösungsmittel | Dichloromethane | HCID 6344 | — |
| Produkt | 2,3-Dihydroxy-4-methoxybenzaldehyde | HCID 11557352 | 73% |
Reaktionsschritte
A dry CH2Cl2 (200 mL) solution of 2,3,4-trimethoxybenzaldehyde (19.6 g, 100 mmol), under nitrogen, was stirred for 10 min and BCl3 (1.0M solution in CH2Cl2, 200 mL) was added. The reaction was stirred for 24 hours and a 10% sodium bicarbonate solution (40 g/360 mL) was added. The resulting solution was acidified with concentrated HCl to PH 1. The organic layer was separated, and the aq. layer was extracted with EtOAc (4×100 mL). The organic layer was dried with MgSO4 and filtered through celite. After solvent evaporation, the crude mixture was recrystallized using (Hexanes/EtOAc:70/30) to afford 12.2 g (72.6 mmol, 73%) of a purple solid.
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US07091240B2 |
| Quelldatensatz | uspto-grants-2006_08 |
| ORD ID | ord-9c5bd52821714c9bb9e8153a9d33262f |
| Quellennotiz | uspto-grants-2006_08 |