HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
Methanol → 2,3-Difluoro-6-(hydroxymethyl)phenol
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | Methanol | HCID 887 | — |
| Edukt | Dimethyl Sulfide | HCID 1068 | — |
| Edukt | 3,4-Difluoro-2-hydroxybenzoic acid | HCID 2758286 | — |
| Lösungsmittel | Tetrahydrofuran | HCID 8028 | — |
| Produkt | 2,3-Difluoro-6-(hydroxymethyl)phenol | HCID 45119104 | 91,7% |
Reaktionsschritte
To a solution of 3,4-difluoro-2-hydroxy benzoic acid (3.2 g 18.39 mmol) in THF (20 mL) was added BH3.Me2S (7 mL 73.56 mmol) drop wise, over a period of 20 min. at RT. The reaction mixture was stirred at RT for 3 h and monitored by TLC. Methanol (20 mL) was added and the solvent was removed under vacuum. The crude compound was purified by column chromatography over silica gel using a mixture of ethyl acetate and hexane (20:80) as eluent to give the alcohol (2.7 g, 91% yield) MS: m/z 159 (M+1).
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US07902394B2 |
| Quelldatensatz | uspto-grants-2011_03 |
| ORD ID | ord-a2feb40b64ad4e109c672ebbd701c6e6 |
| Quellennotiz | uspto-grants-2011_03 |