HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
6-Hydroxy-3-methyl-4-vinyl-phthalic Acid Dimethyl Ester → 4-Ethyl-6-hydroxy-3-methyl-phthalic Acid Dimethyl Ester
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | 6-Hydroxy-3-methyl-4-vinyl-phthalic Acid Dimethyl Ester | HCID 59794498 | — |
| Lösungsmittel | Benzene | HCID 241 | — |
| Lösungsmittel | Ethyl Acetate | HCID 8857 | — |
| Produkt | 4-Ethyl-6-hydroxy-3-methyl-phthalic Acid Dimethyl Ester | HCID 59794477 | 88,4% |
Reaktionsschritte
6-Hydroxy-3-methyl-4-vinyl-phthalic acid dimethyl ester (1.27 g, 5.11 mmol) was dissolved in benzene (10 mL) and EtOAc (10 mL). Tristriphenylphosphine rhodium chloride (150 mg) was added and the reaction was placed under an atmosphere of hydrogen. Stirring at room temperature was continued. After 14 hours, the solvents were removed in vacuo and the crude material was purified by silica gel chromatography to provide 1.14 g (88%) of the desired product as an off-white solid. 1H NMR (300 MHz, CDCl3): δ=1.19 (t, J=7.8 Hz, 3H), 2.10 (s, 3H), 2.60 (q, J=7.8 Hz, 2H), 3.89 (s, 6H), 6.87 (s, 1H), 10.79 (s, 1H) ppm.
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US07452901B2 |
| Quelldatensatz | uspto-grants-2008_11 |
| ORD ID | ord-f030c0e328744626b6a9d1e4a949d794 |
| Quellennotiz | uspto-grants-2008_11 |